Formation Of Bimetallic Nanoparticles Research Articles

Direct Observation of Hollow Bimetallic Nanoparticle Formation through Galvanic Replacement and Etching Reactions.

Hollow bimetallic nanoparticles (NPs) formed from metal oxide NP templates are widely used catalysts for hydrogen evolution and CO2 reduction reactions. Despite their importance in catalysis, the details of how these NPs form on the NP templates remain unclear. Here, using in situ liquid-phase transmission electron microscopy (TEM) imaging, we describe the conversion of Cu2O template NPs to hollow PdCu NPs. Our observations show that a polycrystalline PdCu shell forms on the surface of the template via a galvanic replacement reaction while the template undergoes anisotropic etching. This study provides important insights into the synthesis of hollow metallic nanostructures from metal oxide templates.

Recyclable Cu–Ag bimetallic nanocatalyst for radical scavenging, dyes removal and antimicrobial applications

An ecofriendly and cost effective green method has been used for the synthesis of recyclable, high functional nanoparticles. Bimetallic nanoparticles (BmNPs), Cu–Ag, have been synthesized using beetroot extract as reducing and capping agent. Formation of BmNPs was initially confirmed by UV–visible analysis, having distinct peaks of Ag at 429 nm and Cu at 628 nm. FTIR analysis also confirmed the association of bioactive phytochemicals with Cu–Ag nanoparticles. Crystallinity and morphology of BmNPs was determined through X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), dynamic light scattering (DLS) and energy dispersion X-ray spectroscopy (EDAX). The size of spherical shape Cu–Ag BmNPs was found to be 75.58 nm and EDAX studies confirmed the percent elemental composition of Cu and Ag in synthesized nanocatalyst. Results of different analysis provided supported evidences regarding the formation of BmNPs. Catalytic potential of BmNPs was tested for the degradation of rhodamine B (Rh–B), methylene blue (MB) and methyl orange (MO) dyes. Cu–Ag BmNPs exhibited outstanding catalytic activity for the degradation of selected organic dyes and percent degradation was recorded more than 90% for each dye. In addition, antiradical property of BmNPs was tested employing DPPH● and ABTS●+ assays and it was found to be promising. Synthesized BmNPs also exhibited strong antimicrobial activity against Salmonella typhimurium and Bacillus subtilis. Recyclability of nanoparticles was also evaluated and recovery from dye degradation reaction mixture was successfully achieved. The recovered nanoparticles exhibited same catalytic potential for the degradation of Rh–B. The objective of the current study was to synthesize BmNPs Cu–Ag employing a cost effective green method having promising catalytic, antiradical and antimicrobial potential. Further, BmNPs were reused after recovery from catalytic reactions, proving that BmNPs can be recycled having the same efficiency as that of a freshly prepared Cu–Ag BmNPs.

Electrochemical Activation Applied to Perovskite Titanate Fibers to Yield Supported Alloy Nanoparticles for Electrocatalytic Application.

Active bi-metallic nanoparticles are of key importance in catalysis and renewable energy. Here, the in situ formation of bi-metallic nanoparticles is investigated by exsolution on 200nm diameter perovskite fibers. The B-site co-doped perovskite fibers display a high degree of exsolution, decorated with NiCo or Ni3 Fe bi-metallic nanoparticles with average diameter about 29 and 35nm, respectively. The perovskite fibers are utilized as cathode materials in pure CO2 electrolysis cells due to their redox stability in the CO/CO2 atmosphere. After in situ electrochemical switching, the nanoparticles exsolved from the perovskite fiber demonstrate an enhanced performance in pure CO2 electrolysis. At 900°C, the current density of solid oxide electrolysis cell (SOEC) with 200µm YSZ electrolyte supported NiFe doped perovskite fiber anode reaches 0.75Acm-2 at 1.6V superior to the NiCo doped perovskite fiber anode (about 1.5 times) in pure CO2 . According to DFT calculations (PBE-D3 level) the superior CO2 conversion on NiFe compared to NiCo bi-metallic species is related to an enhanced driving force for C-O cleavage under formation of CO chemisorbed on the nanoparticle and a reduced binding energy of CO required to release this product.

Valorization of Parkia biglobosa wastewater for novel biofabrication of Ag/TiO2 nanoparticles with potent action against MDR strains and nanotextile application

In this work, we report for the first time, the biogenic production of silver-titanium oxide alloy nanoparticles (Ag/TiO2 NPs) via wastewater from fermented beans of locust beans plant (Parkia biglobosa) with potent antimicrobial activities using as-prepared nanoparticles and fabric functionalized with the nanoparticles. The deep brown colloidal solution of Ag/TiO2 NPs absorbed at 400 nm with a single peak that signifies the formation of bimetallic nanoparticles. The characteristic peaks of 3898–3900, 3493–3506 and 1773–1775 cm−1 obtained through Fourier Transform Infrared spectroscopic investigations showed the involvement of proteins and phenolics in the synthesis of Ag/TiO2 NPs. The transmission electron microscopic measurement of the nearly spherical-shaped nanoparticles revealed size range of 11.40–28.93 nm with crystalline structure in the selected area electron diffraction (SAED) image. The energy-dispersive X-ray pattern showed prominence of silver, oxygen and titanium in the colloidal solution. The synthesized Ag/TiO2 NPs inhibited the growth of strains of multi-drug resistant bacteria such as Klebsiella oxytoca, Pseudomonas aeruginosa, Staphylococcus aureus, Proteus mirabilis, Klebsiella pneumoniae, and Escherichia coli as well as fungal isolates that included Aspergillus niger, Aspergillus flavus, Aspergillus fumigatus and Fusarium solani. Similarly, the antimicrobial potency of the fabrics functionalized with Ag/TiO2 NPs NPs was remarkable with antibacterial activities (15–24 mm) and complete suppression of the growth of A. niger. This novel antimicrobial agent can be explored for textile and biomedical applications in the control of drug resistant isolates to engender good health and wellbeing (SDG 3).

Biosynthesized Bimetallic (ZnOSnO2) Nanoparticles for Photocatalytic Degradation of Organic Dyes and Pharmaceutical Pollutants

The quest for eco-friendly synthetic routes that can be used for the development of multifunctional materials, in particular for water treatment, has reinforced the use of plant extracts as replacement solvents. In this study, bimetallic ZnOSnO2 nanoparticles of different ratios were synthesized using the Sutherlandia frutescens (S. frutescens) plant and tested for the degradation of methylene blue dye and the antibiotics sulfisoxazole and sulfamethoxazole. From the analysis, FTIR confirmed the formation of bimetallic nanoparticles in all ratios within the fingerprint region. SEM revealed homogenous and heterostructures of tubular and spherical structures, with the size distribution ranging from 5–60 nm, respectively. XRD confirmed the formation and the crystallinity of the bimetallic nanoparticles, UV-Vis confirmed the optical properties of the materials and the bandgap values were found between 3.08 and 3.3 eV. From the surface area analysis, type III isotherm and mesoporous structures were confirmed. The photocatalytic activity of these ratios was investigated against MB dye and the antibiotics SSX and SMX. The highest degradation of 88% for MB was obtained using the 50:50 loading ratio at 150 min with a fast kinetic rate of 0.0008 min−1. Furthermore, the holes were the species found to be responsible for the degradation of MB. The SSX and SMX antibiotics exhibited a 66% and 70% degradation, respectively. From this analysis, it can be noted that it is possible to synthesize environmentally safe materials that can be used to degrade various pollutants in our water streams.

Control of cluster coalescence during formation of bimetallic nanoparticles and nanoalloys obtained via electric explosion of two wires

In this study, the possibility of controlling the coalescence of clusters during the formation of bimetallic nanoparticles and nanoalloys is demonstrated for the first time using joint electric explosion of Nb/Al and Nb/Ag wires under an argon atmosphere as an example. The evolution of clusters in the condensed phase is considered based on the adiabatic approximation to expand the products of the electric explosion of wires. Controlling the temperature and size of the clusters formed under the electric explosion of wires generating the energy necessary for the transition from the metallic state to the two-phase state (clusters of the condensed phase and weakly ionized plasma) allows synthesizing nanoparticles and bimetallic nanoparticles possessing the structures of nanoalloys and Janus particles, respectively. The experimental studies are supplemented by describing structural patterns and segregation phenomena using a hybrid computer experiment that adopts two alternative methods, i.e., the Monte Carlo and molecular dynamics methods. Both methods predict similar structure formation trends, particularly segregation patterns, in Nb–Ag and Nb–Al nanoparticles. For the first time, we have obtained bimetallic nanoparticles possessing a more complex structure, compared to the formerly known core shell, namely the onion-like structure. The Nb2964–Ag2964 and Nb2964–Al2964 nanoparticles s are characterized by the formation of icosahedral cores and crystalline cores based on the hcp and fcc phases, respectively, over the entire temperature range studied.

Low-Temperature Exsolution of Ni-Ru Bimetallic Nanoparticles from A-Site Deficient Double Perovskites.

Exsolution of stable metallic nanoparticles for use as efficient electrocatalysts has been of increasing interest for a range of energy technologies. Typically, exsolved nanoparticles show higher thermal and coarsening stability compared to conventionally deposited catalysts. Here, A-site deficient double perovskite oxides, La2- x NiRuO6- δ (x=0.1and 0.15), are designed and subjected to low-temperature reduction leading to exsolution. The reduced double perovskite materials are shown to exsolve nanoparticles of 2-6nm diameter during the reduction in the low-temperature range of 350-450°C. The nanoparticle sizes are found to increase after reduction at the higher temperature (450°C),suggestingdiffusion-limited particle growth. Interestingly, both nickel and ruthenium are co-exsolved during the reduction process. The formation of bimetallic nanoparticles at such low temperatures is rare. From the insitu impedance spectroscopy measurements of the double perovskite electrode layers, the onset of the exsolution process is found to be within the first few minutes of the reduction reaction. In addition, the area-specific resistance of the electrode layers is found to decrease by 90% from 291to 29Ωcm2 , suggesting encouraging prospects for these low-temperature rapidly exsolved Ni/Ru alloy nanoparticles in a range of catalytic applications.

Pt-Fe nanoalloy: Structure evolution study and catalytic properties in water gas shift reaction

In the present work we studied the properties of Pt0.5Cu0.5, Pt0.5Fe0.5, Pt0.33Ag0.67, Pt0.6Au0.4 nanoalloys in water gas shift (WGS) reaction for the first time. Cu, Fe, Ag, Au were chosen as modifiers due to the low catalytic activity in undesirable side reactions of carbon oxides methanation. Nanoalloys were synthesized via corresponding double complex salts decomposition, which provided the selective formation of bimetallic nanoparticles. A simulated reformate gas mixture, containing (vol.%) 10 CO, 15 CO2, 30 H2O and 45 H2, was used to evaluate the activity of these systems. Only Pt0.5Fe0.5 nanopowder was active, while Pt-FeOx metal-oxide composite was inert. The positive effect of Pt-Fe alloying on WGS performance was also confirmed for silica supported catalysts. TG and XRD in situ analysis reveal that Pt0.5Fe0.5 is stable toward oxidation under WGS reaction conditions (T < 350°C, reductive atmosphere), while Pt-FeOx undergoes partial reduction but without formation of Pt-Fe alloy nanoparticles.

Antioxidant and Organic Dye Removal Potential of Cu-Ni Bimetallic Nanoparticles Synthesized Using Gazania rigens Extract

Copper-nickel bimetallic nanoparticles (Cu-Ni BNPs) were fabricated using an eco-friendly green method of synthesis. An extract of synthesized Gazania rigens was used for the synthesis of BNPs followed by characterization employing different techniques including UV/Vis spectrophotometer, FTIR, XRD, and SEM. Spectrophotometric studies (UV-Vis and FTIR) confirmed the formation of bimetallic nanoparticles. The SEM studies indicated that the particle size ranged from 50 to 100 nm. Analysis of the BNPs by the XRD technique confirmed the presence of both Cu and Ni crystal structure. The synthesized nanoparticles were then tested for their catalytic potential for photoreduction of methylene blue dye in an aqueous medium and DPPH radical scavenging in a methanol medium. The BNPs were found to be efficient in the reduction of methylene blue dye as well as the scavenging of DPPH free radicals such that the MB dye was completely degraded in just 17 min at the maximum absorption of 660 nm. Therefore, it is concluded that Cu-Ni BNPs can be successfully synthesized using Gazania rigens extract with suitable size and potent catalytic and radical scavenging activities.

Use of single particle inductively coupled plasma mass spectrometry for understanding the formation of bimetallic nanoparticles

Bimetallic nanoparticles (NPs), including core-shell structure and bimetallic alloy nanoparticles, were synthesized and characterized using flow field-flow fractionation (FlFFF), single particle inductively coupled plasma mass spectrometry (SP-ICP-MS), and transmission electron microscope (TEM) with energy-dispersive x-ray spectroscopy (EDS). For the core-shell particles, a nominal 80 nm commercial core-shell AuAg bimetallic nanoparticle was used to examine the applicability of SP-ICP-MS to determine the core size of Au and shell thickness of Ag. Then, the method was applied to estimate the core size of Au and shell thickness of Ag for the laboratory synthesized particles. The results were compared with those obtained from TEM-EDS. For the alloy nanoparticles, two synthesis protocols, based on the galvanic replacement of Ag seed particles with Au, were used. One was to prepare a hollow AgAu particle by varying the volume of dissolved Au in basic solution (K-gold) to etch some parts of AgNPs to dissolved ionic silver with the formation of AuNPs covering the remaining AgNPs, producing a hole inside the core nanoparticles. Another protocol was to prepare AgAu alloy nanoparticles. SP-ICP-MS was used in combination with FlFFF to provide information on the changes of particle size with varying volume of K-gold reagent. Hydrodynamic diameter increased with increasing K-gold, as observed by FlFFF. With SP-ICP-MS without prior FlFFF, bimodal distributions were observed in the size distribution of Au and Ag. With prior FlFFF, monomodal distributions were observed by SP-ICP-MS, which allow the use of particle concentration and size to estimate the mass concentration of elements on the fractionated bimetallic nanoparticles. This study illustrates the potential use of SP-ICP-MS for gaining information about particle transformation during the synthesis of bimetallic nanoparticles.

Preparation and Investigation of Pd and Bimetallic Pd-Sn Nanocrystals on γ-Al2O3

One of the key factors for producing highly dispersed controlled nanoparticles is the method used for metal deposition. The decomposition of metal-organic precursors is a good method for deposition of metal nanoparticles with very small sizes and narrow size distributions on the surface of various supports. The preparation process of Pd and bimetallic Pd-Sn nanoparticles supported onto γ-Al2O3 is considered. The samples were prepared by diffusional co-impregnation of the γ-Al2O3 support by using organometallic Pd(acac)2 and Sn(acac)2Cl2 precursors. To achieve the formation of Pd and bimetallic Pd-Sn nanoparticles on the support surface, the synthesized samples were then subjected to thermal decomposition under Ar (to decompose the organometallic bound to the surface while keeping the formed nanoparticles small) followed by an oxidation in O2 (to eliminate the organic compounds remaining on the surface) and a reduction in H2 (to reduce the nanoparticles oxidized during the previous step). A combination of methods (ICP-OES, TPR-H2, XPS, TEM/EDX) was used to compare the physical-chemical properties of the synthesized Pd and bimetallic Pd-Sn nanoparticles supported on the γ-Al2O3. The three samples exhibit narrow size distribution with a majority on nanoparticles between 3 and 5 nm. Local EDX measurements clearly showed that the nanoparticles are bimetallic with the expected chemical composition and the measured global composition by ICP-OES. The surface composition and electronic properties of Pd and Sn on the γ-Al2O3 support were investigated by XPS, in particular the chemical state of palladium and tin after each step of thermal decomposition treatments (oxidation, reduction) by the XPS method has been carried out. The reducibility of the prepared bimetallic nanoparticles was measured by hydrogen temperature programmed reduction (TPR-H2). The temperature programmed reduction TPR-H2 experiments have confirmed the existence of strong surface interactions between Pd and Sn, as evidenced by hydrogen spillover of Pd to Sn (Pd-assisted reduction of oxygen precovered Sn). These results lead us to propose a mechanism for the formation of the bimetallic nanoparticles.

Synthesis and Application of FeCu Bimetallic Nanoparticles in Coal Mine Wastewater Treatment

Wastewater treatment has become a global challenge with wastewater treatment cost fast increasing. Industrial processes such as downstream processes, wastewater treatment, and several fermentation processes depend largely on the use of flocculants. Synthetic flocculants, which are conventionally used in wastewater treatment, are hazardous to the environment and are carcinogenic to human health. Therefore, bioflocculants can be used as an alternative due to their biodegradable and environmentally friendly nature. However, low efficacy hinders their industrial application. This necessitates the need for a new technology to combat wastewater treatment challenges. Nanotechnology provides the platform to explore the possible solutions to these problems. The combination of two different metals results in the formation of bimetallic nanoparticles (BNPs). Due to better properties, bimetallic nanoparticles have attracted huge attention as compared to monometallic nanoparticles from both technological and scientific views. Iron copper bimetallic nanoparticles (FeCu BNPs) were successfully stabilized by bioflocculant and used in the coal mine wastewater treatment. Infrared spectrometric analysis showed the presence of carboxyl (COO−), hydroxyl (−OH), and amino (−NH2) functional groups. SEM images showed irregular and crystalline like morphology. Meanwhile, TEM analysis revealed chain like agglomerated nanoparticles. FeCu BNPs exhibited a wide pH stability range from 3, 7, and 11 with 99% flocculation activity at pH 7 and at lowest dosage of 0.2 mg/mL. After treating wastewater, the FeCu BNPs could remove pollutants such as phosphate, sulfate, calcium, chemical oxygen demand (COD), and biological oxygen demand (BOD) with phosphate having the highest removal efficacy of 99%.

Bimetallic nanoparticle generation from Au − TiO2 film by pulsed laser ablation in an aqueous medium

Bimetallic nanoparticle formation by applying pulsed laser ablation on the gold (Au) - titanium (TiO2) film was demonstrated. Experiments were conducted at room temperature. Au and TiO2 nanoparticles were mixed in different ratios and deposited as the starting material on silicon wafer plates, which were dried and placed in a beaker with distilled water. After a pulsed laser beam was applied, the collected aqueous solution products were analysed by ultraviolet–visible (UV–vis) spectrophotometry and characterised by scanning transmission electron microscopy (STEM) with energy-dispersive X-ray spectroscopy (EDS). The UV spectra indicated that the Au, TiO2, and Au–TiO2 nanoparticles were dispersed in the aqueous solution product. STEM-EDS images showed that spherical bimetallic nanoparticles containing gold and titanium were generated. A core of TiO2 nanoparticles was found to be well surrounded by a shell of Au nanoparticles when colloidal Au and TiO2 nanoparticles at a 1:1 ratio was used as the starting materials. The technique described here is simple and innovative, and this study enhances our understanding of bimetallic nanoparticle synthesis using a pulsed laser beam in a liquid environment.

Bio-Fabrication, Spectroscopic Investigation and Antibacterial Potency of Ag-Co Bimetallic Nanoparticles Synthesized from the Root Extract of Borassus aethiopum (Palmyra Palm)

In this study, silver-cobalt bimetallic hybrid nanoparticles were synthesized using green method from AgNO3 and CoCl2 metal precursors as well as the locally available root extract of Borassus aethiopum acting as the reducing agent. The formation of bimetallic nanoparticles was first noticed by a color change of the reaction mixture from light pink to light brown as the result of Surface Plasmon absorptions. The optical measurements using UV-Vis showed the maximum absorption wavelength at 420nm while the functional group identification using FT-IR revealed some replacements in the absorption of functional groups, disappearance, and appearance of some others in the spectra of the BMNPs relative to that of the root extract indicating that those involved in the bio-reduction process. In vitro antibacterial potency was investigated against five clinically isolated bacteria. The outcome of the result suggested that they inhibit the tested bacteria especially against Salmonella typhi, Bacillus subtilis and Klebsiella pneumoniae. Thus, it can be developed as a bio-control agent for the treatment of diseases caused by these bacterial pathogens.

Catalytically active PdRu and CuRu bimetallic nanoparticle formation in the mesoporous SiO2 by supercritical CO2-assisted immobilization

In the past decade, the use of bimetallic nanoparticles (NPs) as catalytic systems has demonstrated to be an effective method to overcome the unfortunate shortage of expensive Pd-like metals. These NP systems exbibit excellent catalytic activities. In this paper, we present a method to immobilize PdRu and CuRu NPs in the mesopores of hierarchical porous SiO2 using a supercritical CO2 (scCO2) solution, employing commonly available metal-organic complexes as feed materials. Scanning TEM coupled with electron dispersive X-ray spectroscopy (STEM-EDX) revealed the homogeneous distribution of the single metal components in the NPs. The resulting PdRu@SiO2 and CuRu@SiO2 systems exhibited higher activities for CO oxidation than those of monometallic Pd@SiO2, Ru@SiO2, and Rh@SiO2. Our results show that coupling Ru with Pd or Cu in nanosized structures can afford excellent catalytic systems at a lower cost compared to that of their monometallic counterparts.

Anti-proliferative and anti-migratory effects of flower-like bimetallic (Au@Pt) nanoparticles

In this work, flower-like bimetallic (Au@Pt) nanoparticles were synthesized by using Carica papaya leaf extract. The optical, structural, and functional properties have been investigated. The UV–vis spectra inferred the formation of bimetallic nanoparticles with highly ordered crystalline structure as revealed by X-ray diffraction analysis. The TEM micrography revealed flower-like bimetallic nanoparticles of 150 ± 1.02 nm. The cytotoxicity of bimetallic nanoparticles was confirmed against MCF-7 breast cancer cells, which indicates their anti-proliferative effect (IC50 value − 120 ± 2.32 µg mL−1). The developed flower-like bimetallic nanoparticles also displayed anti-migration effect by wound healing assay, making it sensibly valuable for cancer chemotherapy.

Закономерности формирования структурно-фазовых состояний биметаллических наночастиц Ag-Cu, полученных электрическим взрывом двух проволок

In present work we observed structural phase state formation of Ag-Cu nanoparticles by electrical explosive of wires. We observed the formation of bimetallic nanoparticles with a number average size of 75 ... 82 nm by synchronous and nonsynchronous electric explosion of wires. The phase composition of the samples is represented by phases based on solid solutions of copper and silver. The results of the studies allow us to conclude that, using electric explosion of copper and silver wires, bimetallic Ag-Cu nanoparticles with different mass ratio of metals can be obtained.

Nanoalloying of clusters of immiscible metals and the formation of bimetallic nanoparticles in the conditions of non-synchronous explosion of two wires

The work researches the influence of metal mixing enthalpy on spontaneous nanoalloying of coagulated clusters formed when intertwined Fe/Ag, Ni/Ag, Nb/Сu and Pb/Сu wires with equiatomic composition are exploded. The analysis of temporal dependencies of currents and voltages has shown that the intervals between the successive explosions of Fe/Ag, Ni/Ag, Nb/Сu and Pb/Сu wires are 0.38, 0.26, 0.43 and 0.4 μs, respectively. This explains their asynchronous destruction. It has been found that when wires are exploded, bimetallic Janus and core-shell nanoparticles are formed. The obtained data makes it possible to conclude that when wires explode non-synchronously, clusters coagulate and atoms of metals subsequently intermix. The results of the research demonstrate that the explosion of two wires made of metals with positive mixing enthalpy (from 8 to 116 kJ/g) is a process that can be used to obtain bimetallic nanoparticles with complex structures.

Formation and Functioning of Bimetallic Nanocatalysts: The Power of X‐ray Probes

AbstractBimetallic nanocatalysts are key enablers of current chemical technologies, including car exhaust converters and fuel cells, and play a crucial role in industry to promote a wide range of chemical reactions. However, owing to significant characterization challenges, insights in the dynamic phenomena that shape and change the working state of the catalyst await further refinement. Herein, we discuss the atomic‐scale processes leading to mono‐ and bimetallic nanoparticle formation and highlight the dynamics and kinetics of lifetime changes in bimetallic catalysts with showcase examples for Pt‐based systems. We discuss how in situ and operando X‐ray spectroscopy, scattering, and diffraction can be used as a complementary toolbox to interrogate the working principles of today's and tomorrow's bimetallic nanocatalysts.

Formation and Functioning of Bimetallic Nanocatalysts: The Power of X-ray Probes.

Bimetallic nanocatalysts are key enablers of current chemical technologies, including car exhaust converters and fuel cells, and play a crucial role in industry to promote a wide range of chemical reactions. However, owing to significant characterization challenges, insights in the dynamic phenomena that shape and change the working state of the catalyst await further refinement. Herein, we discuss the atomic‐scale processes leading to mono‐ and bimetallic nanoparticle formation and highlight the dynamics and kinetics of lifetime changes in bimetallic catalysts with showcase examples for Pt‐based systems. We discuss how in situ and operando X‐ray spectroscopy, scattering, and diffraction can be used as a complementary toolbox to interrogate the working principles of today's and tomorrow's bimetallic nanocatalysts.