X-ray Photoelectron Spectroscopy Methods Research Articles

Participation of Surface Oxygen in the Stabilization of the Rh/HOPG System with Respect to NO₂

In this work, using the method of X-ray photoelectron spectroscopy (XPS), a comparative study of the nature of the interaction of NO₂ at room temperature and a pressure of 10⁻⁵ mbar with two samples of highly oriented pyrolytic graphite (HOPG), on the surface of which rhodium was preliminarily deposited by vacuum deposition, was carried out. Before metal deposition, one of the HOPG samples was annealed in vacuum at 600°C, and the other was subjected to bombardment with argon ions, followed by exposure to air at room temperature for an hour in order to introduce strongly bound oxygen atoms into the surface composition. After deposition of rhodium on two samples of HOPG prepared, two model catalysts were obtained, designated as Rh/C and Rh/C(A)-O. It was found that the interaction of NO₂ with Rh/C led to the oxidation of graphite with the destruction of the surface layer. The Rh particles remained in the metallic state, but at the same time they were introduced into the near-surface layer of the carbon support. On the contrary, when the Rh/C(A)-O sample was treated with NO₂, the deposited rhodium was partially converted into RH₂O₃, while the graphite was oxidized to an insignificant degree and retained its original structure. The role of surface oxygen in the stabilization of graphite with respect to oxidation to NO₂ was discussed.

Influence of N 2, N 6-bis((3,5-dimethyl-1h-pyrazol-1-yl)methyl) pyridine-2,6-diamine on C35E steel corrosion in 1 M HCl medium: Experimental and theoretical studies

The inhibition effect of N 2, N 6-bis((3,5-dimethyl-1H-pyrazol-1-yl)methyl)pyridine-2,6-diamine (MH-PA) on the corrosion of C35E steel in 1 M HCl solution was investigated employing potentiodynamic polarization (PDP), electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), Fourier-transform infrared (FTIR) spectroscopy, atomic force microscopy (AFM), contact angle, X-ray photoelectron spectroscopy (XPS) methods, UV-visible spectroscopy, and theoretical calculation methods. The inhibition efficiency increased with increasing MH-PA concentration and decreased with increasing temperature, attaining 98% inhibition efficiency at 10−3M under 303K. PDP studies indicated that MH-PA is a mixed-type corrosion inhibitor and its adsorption mode conforms to Langmuir isotherm. UV-visible and FTIR spectroscopy support MH-PA adsorption over the C35E steel surface. The surface analysis through SEM, EDS, AFM, and contact angle corroborates the formation of the protective layer of MH-PA molecules on the C35E steel surface. In addition, XPS analysis revealed the formation of an N-Fe bond. Thermodynamic properties revealed that MH-PA has both physical and chemical adsorption behavior. Molecular dynamics simulations manifest that MH-PA molecules adsorb parallel to the Fe (110) surface.

Indium-nickel oxide nanocomposite for room temperature H2 gas detection and its sensing mechanism

Lithium-ion batteries (LIBs) have a wide range of applications in energy storage power stations. However, thermal runaway of LIBs can lead to serious safety accidents and cause significant losses. Therefore, it is particularly important to carry out early security warning of LIBs. And H2 is generated along with the growth of lithium dendrites, which can serve as an effective indicator for detecting LIBs before TR. In this paper, In2O3/NiO nanocomposites were prepared, and five groups of samples were systematically prepared by adjusting the molar ratio of In and Ni. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and other test methods were used to characterize the prepared nanocomposites. Through experiments, the best samples among several groups of samples were determined. When the test gas is introduced, the resistance change of this optimal sensor is the greatest, indicating the best performance, which is significantly better than pure In2O3 and pure NiO samples. Furthermore, compared to other gases, this nanocomposite sensor exhibits significant selectivity towards H2. The results show that In2O3/NiO is a promising candidate material for room temperature H2 detection, and provide suggestions for the development of gas sensors with heterogeneous structures.

S-scheme TiO2/Bi2WO6 heterojunction for enhanced photocatalytic selective oxidation of toluene

Selective activation of saturated C-H bonds in hydrocarbons, such as the activation of the C-H bond in toluene, is an effective method for the production of high value-added chemicals. However, improving the C-H bond activation of toluene remains a challenge. In this study, S-scheme TiO2/Bi2WO6 composites were synthesized by loading TiO2 nanoparticles on Bi2WO6 flakes using a simple hydrothermal method. The physical and chemical properties of the prepared materials were characterized using X-Ray Diffraction (XRD), Fourier Transform Infrared Spectoscopy (FT-IR), Scanning Electronic Microscopy (SEM), X-ray Photoelectron Spectroscopy (XPS) and other characterization methods. Selective oxidation of toluene to benzaldehyde under visible light irradiation using air as an oxidizing agent. When the molar ratio of TiO2 and Bi2WO6 was 0.20, the composites exhibited excellent photocatalytic performance with a benzaldehyde production rate of 1725.41 μmol·g-1·h-1, which was 2.31 and 1.91 times higher than that of TiO2 and Bi2WO6, respectively. This excellent performance is attributed to the formation of heterojunction structure by the loaded TiO2 nanoparticles, which improves the separation efficiency of photogenerated carriers and thus enhances its photocatalytic performance. In addition, the active substances involved in the photocatalytic reaction were identified by free radical trapping experiments as ·O2- and h+. Finally, the photocatalytic mechanism of S-scheme TiO2/Bi2WO6 composites was proposed by energy band structure analysis and radical trapping experiments. This study provides a simple design pathway for the construction of visible-light responsive bismuth tungstate-based heterojunction photocatalysts and some ideas for the development of new and efficient photocatalytic toluene selective oxidation catalysts.

Direct electrocatalytic sensing of myoglobin using an annealed Au-implanted electrode

Ion implantation is a versatile and green material surface modification technology that modifies the structure of target-neat surface by bombardment of non-metal or heavy metal ions. A new Au nanoparticle loaded ITO (AuNPs/ITO) electrodes was prepared by ion implantation and thermal annealing method in this work. The obtained nanoparticles were characterized by Scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS) and electrochemical methods. The direct electrocatalysis of Myoglobin (MB) was reported. It was found that after annealing at 500 °C for 2 h, the damage part of the implanted sample was eliminated. The surface coverage of MB on the MB/AuNPs/ITO electrode and the MB/annealed-AuNPs/ITO electrode was 4.35× 10−11 mol·cm−2 and 1.23 × 10−10 mol·cm−2, respectively. The results show that this composite method can be used to fabricate an electrocatalytic biosensor.

Palladium nanocubes-mediated Fenton catalysis combined with chloride ion-amplified electro-driven catalysis for dye degradation

Electrochemical technology is frequently used to treat industrial dye wastewater. However, its degradation efficiency is restricted by pH, and the low current efficiency and high energy consumption limit its broader application. Based on this, we constructed an innovative electro-driven catalytic system by integrating nanotechnology with electric current. This system operates without pH constraints, has low energy consumption, and allows for the recycle and reuse of both electrodes and catalysts. Firstly, we synthesized palladium (Pd) cubes via a solvothermal method, and characterized their morphology, structural composition, and crystalline properties using transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and other methods. The prepared Pd cubes possessed dual catalytic properties of electro-driven catalysis and Fenton catalysis, achieving a synergistic degradation effect under an electric field. Subsequently, the study explored how catalysts dosage, H2O2 concentration, pH and Cl− concentration affect the catalytic rate. The optimized system was able to degrade 99.17 % of MB within 1 h and was effective against various organic pollutants. After five cycles of reuse, the recovered catalysts maintained over 90 % degradation efficiency in decomposing MB. This process realizes efficient degradation with a low concentration of catalysts, offering a novel approach for nanotechnology in wastewater treatment under electro-driven conditions.

Crystal structure, composition and valence state of cations in mixed-valence A1-xCdxMnO3 (A=Pr, La) ceramics

Abstract Complex manganites A1−xCdxMnO3 (A = Pr, La) are synthesized by solid state reaction method. X-ray diffraction, scanning electron microscopy and energy-dispersive analysis are applied to study their crystal structure, surface morphology, elemental and phase composition. X-ray photoelectron spectroscopy (XPS) methods are used to study the charge states of Pr and La cations, as well as to quantify the fractions of coexisting Mn3+ and Mn4+ ions. La3d-, La4d-, Pr4d- и Mn2p-spectra of La3+, Pr3+, Mn3+ and Mn4+ ions are calculated in the isolated–ion approximation with accounting for multiplet splitting and charge transfer effect. Good agreement with the experiment is obtained. The relative fractions of trivalent and tetravalent manganese ions in La0.45Cd0.78Mn0,9O2.86 and Pr0.50Cd0.76Mn0.86O2.88 samples are determined by fitting the Mn2p spectra by superposition of experimental spectra containing only Mn3+, and only Mn4+ ions; they were found to be 0.71Mn3+/0.29Mn4+ and 0.54Mn3+/0.46Mn4+, respectively.

A novel arrangement of active and ultra-stable electrocatalyst based on iron/nickel/cobalt oxy/hydroxides for continuous oxygen evolution from alkaline seawater splitting

This research offers novel ideas for development a new class of materials with enhanced OER kinetics utilizing an easy electrochemical deposition technique. Here, the Ti/CoNiyOx/FeOOH electrocatalyst was prepared in two steps. First, CoNiyOx thin film was anodically electrodeposited on an activated titanium substrate. Then iron oxyhydroxide (FeOOH) nanosheets were cathodically electrodeposited on the first layer. The properties of this electrocatalyst was evaluated and compared with some monolayer electrocatalysts using field emission scanning electron microscopy (FE-SEM), Raman, energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and electrochemical methods. The Ti/CoNiyOx/FeOOH electrode requires an overpotential less than 330 mV at 100 mA/cm2 with Tafel constant of only 23.7 mV/dec for OER. The Ti/CoNiyOx/FeOOH electrode delivered long-term electrochemical stability in a solution containing corrosive chloride ions for more than 90 h at a constant current density of 100 mA/cm2 (with less than 9 % potential increase). Overall seawater splitting using the synthesized Ti/CoNiyOx/FeOOH electrode was performed at a current density of 100 mA/cm2 by a voltage as low as 1.58 V. The exceptional activity was ascribed to the synergistic effects of high electrochemical active sites and appropriate charge transfer ability found in CoNiyOx/FeOOH junction.

NH3-probe X-ray photoelectron spectroscopy method to characterize solid acidity of clay minerals

Accurate determination of solid acidity is essential for evaluating the catalytic activity of clay minerals. However, the conventional Fourier-transform infrared (FTIR) method using NH3 as the probe encounters challenges in measuring the solid acidity owing to the presence of water on the surface or within interlayer spaces of clay minerals as well as the influence of environmental water during the detection process. To mitigate water interference, a NH3-probe X-ray photoelectron spectroscopy (XPS) approach was adopted as an alternative to the FTIR method for the identification and semi-quantification of solid acidity of clay minerals. Following NH3 adsorption, the types of solid acid sites in clay minerals were identified through the chemical shift in N1s XPS spectra. The ratio of Brønsted and Lewis acid sites in a given sample and the relative concentration of acid sites across different samples were determined by examining the specific N1s peak area ratio. According to the XPS data, the ratios of Brønsted and Lewis acid sites in Ca-montmorillonite (SAz-2) and Na-montmorillonite (SWy-2) were nearly 1:1, whereas that for the illite–smectite mixed-layer mineral (ISCz-1) was 4. The acid site contents in SAz-2 were more than twice those of SWy-2. This work highlights the promising application prospects of the NH3-probe XPS method in solid acidity investigations of clay minerals.

Facile purification of glass fiber powder by sedimentation for enhanced epoxy resin composites

Glass fiber powder contains two distinct forms: crumb-shaped and rod-shaped glass fiber powder particles. The shape and size of the particles in glass fiber powder have a great influence on its application. In order to separate rod-shaped glass fiber, the effects of different dispersants, such as SHMP, NaOL, and Na2SiO3 on them were investigated by settling experiments. Zeta potential, X-ray photoelectron spectroscopy (XPS), optical microscope, and other methods were used to analyze the adsorption behavior and settling mechanism. Three-point bending experiment and dynamic mechanical analysis (DMA) were used to evaluate the performance of epoxy resin composites reinforced with the raw glass fiber powder and the rod-shaped glass fiber powder. The results show that SHMP can effectively separate crumb-shaped glass fiber powder and rod-shaped glass fiber powder, leading to a notable increase in sedimentation recovery difference, up to Δ=51.08%. A preferential sedimentation separation mechanism is proposed to elucidate the settling mechanism. When the content of glass fiber powder and rod-shaped glass fiber is 5%, the glass transition temperature shifts significantly towards higher values, leading to the optimum comprehensive mechanical properties of the composites. Compared with the original epoxy resin, the flexural strength increased by 10.38% to 95.18 MPa and by 20.11% to 103.57 MPa. Similarly, the storage modulus increased by 14.14% to 2083 MPa and by 21.64% to 2220 MPa.

Optimization of electrical transport and magnetoresistance of La0.72Ca0.28-xPbxMnO3 ceramics by Pb2+ doping

Here, La0.72Ca0.28-xPbxMnO3 (LCPMO, 0 ≤ x ≤ 0.06) polycrystalline ceramics are prepared by the sol-gel method and the influence of Pb2+ doping on microstructure, chemical composition, and electrical transport properties of LCPMO ceramics is systematically investigated. The study was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy-Dispersive Spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and four-probe method. The four-probe test shows that all samples have MIT (metal-insulator transition) behavior, and the peak resistance gradually decreases with the increase of Pb2+ doping amount. With the increase of Pb2+ doping amount, the temperature coefficient of resistance (TCR) and magnetoresistance (MR) first increased and then decreased, the TCR increased from 24.6 % to 36.5 %·K−1, and the MR value increased from 47 % to 71.5 %, and both corresponded to high temperature direction. Referring to previous studies, higher TCR and MR values near room temperature are what researchers have been pursuing for a long time. it can be seen that the LCPMO ceramics prepared in this article can have good application prospects in infrared detection and magnetic storage.

Comparison of the HDS DBT reaction using bulk and supported catalysts

The paper describes in detail the procedure for the preparation of a granular bulk NiMoW catalyst and a supported reference NiMo/Al2O3 catalyst. Mention is made of investigations of the supported and bulk catalysts by various physico-chemical methods (nitrogen adsorption-desorption method, X-ray photoelectron spectroscopy, TPD-NH3, HRTEM and X-ray diffraction analysis). The experiments to estimate catalytic activity and compare rate constant of hydrodesulfurization of dibenzothiophene using both catalysts have been carried out. It is shown that textural properties of the catalysts significantly differ. The supported catalyst has more developed specific surface area and pore volume than the bulk catalyst. TPD-NH3 showed an increased acidity of the supported catalyst in comparison the bulk catalyst. It is shown by the X-ray photoelectron spectroscopy method that in both samples Mo on the surface is present exclusively in the form of Mo4+ ion. However, the bulk catalyst differs from the supported catalyst in that it contains a larger amount of Ni as part of the active NiMo(W)S phase. The catalytic activity tests demonstrated that the bulk catalyst is more active at 240, 250 and 260°C, it is discovered that the rate constant in hydrodesulfurization of dibenzothiophene for the bulk NiMoW catalyst is twice higher at 240ºC than that of the supported NiMo/Al2O3 catalyst.

Effect mechanism of phosphorous-containing additives on carbon structure evolution and biochar stability enhancement

The regulation of the pyrolysis process is a key step in increasing the carbon sequestration capacity of biochar. The effect of K3PO4 addition on the yield, chemical composition, characteristic functional groups, macromolecular skeleton, graphite crystallites, and stability of biochar was studied in this paper using two-dimensional infrared correlation spectroscopy (2D-PCIS), X-ray photoelectron spectroscopy, Raman spectrum, and other characterization methods combined with thermal/chemical oxidation analysis. It is discovered that adding K3PO4 may effectively minimize the graphitization temperature range and increase biochar's yield, aromaticity, H/C ratio, and proportion of refractory/recalcitrant organic carbon. The 2D-PCIS and Raman analysis revealed that K3PO4 mostly promoted the dehydrogenation and polycondensation process of the aromatic rings in the char precursor, transforming the amorphous carbon structure of biochar into an ordered turbostratic microcrystalline structure. K3PO4 enhanced biochar stability mostly at medium-high temperatures (350 ~ 750℃) by stimulating the transformation of unstable structures of biochar to stable carbon-containing structures or by inhibiting the interaction of its active sites with oxidants through the mineralization process. A 20% phosphorus addition increased biochar's refractory index (R50) by roughly 11%, and it also boosted biochar's oxidation resistance (H2O2 or K2CrO4) efficiency, reducing carbon oxidation loss by up to 7.31%. However, at higher temperatures (> 750 ℃), the doping of phosphorus atoms into the carbon skeleton degraded the biochar structure's stability. The results of this study suggest that using exogenous phosphorus-containing additives is an efficient way to improve the stability of biochar.Graphical abstract

Advancing water treatment: Harnessing cyclodextrin metal-organic frameworks with dual protonation sites for enhanced sulfate adsorption efficiency

TTH-CD-MOF was synthesized for sulfate ion adsorption from aqueous solutions, employing cross-linking modification of γ-CD-MOF with N-hydroxyethyl-morpholine as the modifier and triisocyanate as the cross-linking agent. The adsorbent underwent characterization through Fourier transform infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, N2 adsorption-desorption, and other analytical methods. Additionally, the impact of factors such as pH, adsorbent dosage, initial concentration, and ionic strength on adsorption performance was investigated. Adsorption experiments demonstrated the robust efficiency of TTH-CD-MOF for SO42- up to 95.3%, conforming to Langmuir isothermal and pseudo-second-order kinetic models, and higher temperatures favored SO42- adsorption. The maximum adsorption capacity was 189.51 mg·g−1 (25 °C). The adsorption mechanism comprised electrostatic interaction, adsorption within the cavities and pores of γ-CD-MOF. TTH-CD-MOF demonstrates effective sulfate removal from aqueous solutions, establishing its potential as an efficient anion adsorbent.

Electronic structure control of IrO2 via conjugated polymer support for highly efficient oxygen evolution reaction

In this paper, we report synthesis of novel nanoparticle catalyst of iridium oxide supported on conjugated polymer along with evaluation of activity and durability for oxygen evolution reaction. The IrO2/poly(BIAN-thiophene)/TNT catalyst was prepared from iridium complex and poly(BIAN-thiophene)/TNT by hydrothermal method. The synthesized IrO2/poly(BIAN-thiophene)/TNT catalysts was characterized by scanning electron microscopy, transmission electron microscopy, Fourier transfer-infrared spectroscopy, x-ray photoelectron spectroscopy and electrochemical methods. The average particle size of the IrO2 particles on poly(BIAN-thiophene)/TNT was 2.5 nm. The XPS measurement revealed that Ir complex was completely converted to iridium oxide through hydrothermal treatment. The IrO2/poly(BIAN-thiophene)/TNT catalyst showed sufficient performance for OER activity and durability in acidic condition. Our results indicate that IrO2/poly(BIAN-thiophene)/TNT is one of the prospective candidate catalysts for water splitting.

Facile Transfer Hydrogenation of N-Heteroarenes and Nitroarenes Using Magnetically Recoverable Pd@SPIONs Catalyst.

Catalysts with active, selective, and reusable features are desirable for sustainable development. The present investigation involved the synthesis and characterization of bear-surfaced ultrasmall Pd particles (<1 nm) loaded onto the surface of magnetic nanoparticles (8-10 nm). The amount of Pd loading onto the surface of magnetite is recorded as 2.8 wt %. The characterization process covered the utilization of scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), transmission electron microscopy (TEM), inductively coupled plasma (ICP), and X-ray photoelectron spectroscopy (XPS) methods. The Pd@Fe3O4 catalyst has shown remarkable efficacy in the hydrogenation of quinoline, resulting in the production of >99% N-ring hydrogenated (py-THQ) product. Additionally, the catalyst facilitated the conversion of nitroarenes into their corresponding aniline derivatives, where hydrogen was achieved by H2O molecules with the aid of tetrahydroxydiboron (THDB) as an equilibrium supportive at 80 °C in 1 h. The high efficiency of a transfer hydrogenation catalyst is closely related to the metal-support synergistic effect. The broader scope of functional group tolerance is evaluated. The potential mechanism underlying the hydrogenation process has been elucidated through the utilization of isotopic labeling investigations. The application of the heterocyclic compound hydrogenation reaction is extended to formulate the medicinally important tubular polymerization inhibitor drug synthesis. The investigation of the recyclability of Pd@Fe3O4 has been conducted.

Unraveling the evolution of Cathode–Solid electrolyte interface using operando X-ray Photoelectron spectroscopy

Understanding the evolution of the solid electrolyte-electrode interface is currently one of the most challenging obstacles in the development of solid-state batteries (SSBs). Here, we develop an X-ray Photoelectron Spectroscopy (XPS) that allows for operando measurement during cycling. Based on theoretical analysis and the modulated electrode and detector co-grounding mode, the displacement of binding energy can be correlated with the surface electrostatic potential of the material, revealing the charge distribution and composition evolution of the space charge layer between the cathode and the electrolyte. In the investigation of typical LiCoO2 (LCO)/Li6PS5Cl (LPSC)/Li–In batteries, we observed the static potential difference and oxidative decomposition between LPSC and LCO, and the effectiveness of the LiNbO3 coating in reducing potential difference and inhibiting the diffusion of Co and oxidation of S species. Furthermore, our study also revealed that the potential drop between LiNi0·8Co0·1Mn0·1O2 and LPSC is smaller than that of LCO, whilst that between Li3InCl6 and LCO remains near zero. The proposed operando XPS method offers a novel approach for real-time monitoring of interface potential and species formation, providing rational guidance for the interface engineering in SSBs.

A spectroscopic study on the effect of acid concentration on the physicochemical properties of calcined halloysite nanotubes

AbstractHalloysite nanotubes a naturally occurring type of clay with unique properties. This research intends to investigate of the effects of hydrochloric acid treatment on the physicochemical and pore properties of halloysite nanotubes. X-ray diffraction (XRD), field emission scanning electron microscopy (SEM), Fourier-transform infrared (FT-IR) spectroscopy, the nitrogen adsorption-desorption isotherm (BET), thermogravimetric analyses (TGA-DTA) and X-ray photoelectron spectroscopy (XPS) were used to analyze the structure of natural, calcined, and acid-treated calcined halloysite nanotubes. From the analysis of XRD, SEM, FT-IR, BET, and TGA-DTA, it was possible to infer that activation with HCl on the calcined nanotubes allowed for an increase in the specific surface area and the volume of pores while maintaining the tubular structure of these materials. Because the samples’ tubular structure was preserved, the study’s goal was to evaluate the effects of acid treatment on calcined halloysite nanotubes for use as potential adsorbents. The influence of treatment with hydrochloric acid on the structure of halloysite nanotubes calcinated at different temperatures was investigated using a surface sensitive XPS method.

Improved Adhesion of Direct Copper Seed Layer by Medium-Vacuum Sputtering Using Vacuum Ultraviolet Light

A sputtering method is used to form the seed layer for copper electric plating. In general, copper sputtering has weak adhesion to resin, so titanium sputter is combined to increase the adhesion strength. However, etching in the lithography process requires two types of processes, titanium and copper metal. Adhesion strength was improved by performing vacuum ultraviolet (VUV) treatment as a pretreatment for medium-vacuum sputtering. We discovered the relationship between the hydroxyl groups on the resin surface and the adhesion strength by the chemical modification XPS method. Furthermore, by XPS analysis of the peeled copper interface, the adhesion mechanism between the resin and copper due to VUV irradiation was estimated. We evaluated the absorption properties in the vacuum ultraviolet region of a thinly polished glass epoxy resin. We investigated the behavior of functional groups at the interface and considered the effect of vacuum ultraviolet light in the depth direction.

Enhanced removal of copper ions from wastewater using small spherical Fe-N-C material via selective electro-sorption: Experiment and calculation

In the current research, the resource recovery technology for Cu-containing wastewater from electroplating is still a difficult problem. Capacitive deionization technology (CDI) has received widespread attention for its strengths of convenient operation, low cost, and environmentally friendly. In this paper, Fe-N-C was prepared as the electrode material for the treatment of Cu-containing wastewater by capacitive deionization technology through one-pot thermal method. The optimum treatment conditions of Fe-N-C for Cu-containing wastewater were voltage equal to 1 V, pH = 5, and the inlet flow rate was 5 mL/min. The electro-adsorption capacity of a single Cu-containing solution of 400 mg/L could reach 389.4 mg/g. Meanwhile, by carrying out ion competition experiments on five cations, namely Zn2+, Na+, Mg2+, K+, and Cu2+, which demonstrated Fe-N-C had a significant selectivity for the electro-adsorption removal of Cu2+. Theoretical calculations revealed that Fe3N and Fe4N were more dominant for Cu2+ adsorption energy and more binding for competing ions in the monovalent state, but had less practical effect on Cu2+ adsorption. The morphology of the Fe-N-C was analyzed in more depth by X-ray photoelectron spectroscopy (XPS) and other characterization methods. Combined with density functional calculations, Cu would not only displace with Fe in FeXN to form a more stable CuXN structure, but also combine with FeXN to form a Cu-FeXN structure. This is conducive to accelerating the application of CDI to recover Cu2+ from heavy metal wastewater.