Heat Treatment-Induced Microstructure and Property Evolution of Mg/Al Intermetallic Compound Coatings Prepared by Al Electrodeposition on Mg Alloy from Molten Salt Electrolytes

A method of forming an Mg/Al intermetallic compound coating enriched with Mg₁₇Al₁₂ and Mg₂Al₃ was developed by heat treatment of electrodeposition Al coatings on Mg alloy at 350 °C. The composition of the Mg/Al intermetallic compounds could be tuned by changing the thickness of the Zn immersion layer. The morphology and composition of the Mg/Al intermetallic compound coatings were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), and electron backscattered diffraction (EBSD). Nanomechanical properties were investigated via nano-hardness (nHV) and the elastic modulus (EIT), and the corrosion behavior was studied through hydrogen evolution and potentiodynamic (PD) polarization. The compact and uniform Al coating was electrodeposited on the Zn-immersed AZ91D substrate. After heat treatment, Mg₂Al₃ and Mg₁₇Al₁₂ phases formed, and as the thickness of the Zn layer increased from 0.2 to 1.8 μm, the ratio of Mg₂Al₃ and Mg₁₇Al₁₂ varied from 1:1 to 4:1. The nano-hardness increased to 2.4 ± 0.5 GPa and further improved to 3.5 ± 0.1 GPa. The Mg/Al intermetallic compound coating exhibited excellent corrosion resistance and had a prominent effect on the protection of the Mg alloy matrix. The control over the ratio of intermetallic compounds by varying the thickness of the Zn immersion layer can be an effective approach to achieve the optimal comprehensive performance. As the Zn immersion time was 4 min, the obtained intermetallic compounds had relatively excellent comprehensive properties.     

Characterization of Al2O3 Samples and NiAl–Al2O3 Composite Consolidated by Pulse Plasma Sintering

The paper describes an investigation of Al₂O₃ samples and NiAl–Al₂O₃ composites consolidated by pulse plasma sintering (PPS). In the experiment, several methods were used to determine the properties and microstructure of the raw Al₂O₃ powder, NiAl–Al₂O₃ powder after mechanical alloying, and samples obtained via the PPS. The microstructural investigation of the alumina and composite properties involves scanning electron microscopy (SEM) analysis and X-ray diffraction (XRD). The relative densities were investigated with helium pycnometer and Archimedes method measurements. Microhardness analysis with fracture toughness (K_IC) measures was applied to estimate the mechanical properties of the investigated materials. Using the PPS technique allows the production of bulk Al₂O₃ samples and intermetallic ceramic composites from the NiAl–Al₂O₃ system. To produce by PPS method the NiAl–Al₂O₃ bulk materials initially, the composite powder NiAl–Al₂O₃ was obtained by mechanical alloying. As initial powders, Ni, Al, and Al₂O₃ were used. After the PPS process, the final composite materials consist of two phases: Al₂O₃ located within the NiAl matrix. The intermetallic ceramic composites have relative densities: for composites with 10 wt.% Al₂O₃ 97.9% and samples containing 20 wt.% Al₂O₃ close to 100%. The hardness of both composites is equal to 5.8 GPa. Moreover, after PPS consolidation, NiAl–Al₂O₃ composites were characterized by high plasticity. The presented results are promising for the subsequent study of consolidation composite NiAl–Al₂O₃ powder with various initial contributions of ceramics (Al₂O₃) and a mixture of intermetallic–ceramic composite powders with the addition of ceramics to fabricate composites with complex microstructures and properties. In composites with complex microstructures that belong to the new class of composites, in particular, the synergistic effect of various mechanisms of improving the fracture toughness will be operated.     

Manufacturing of Al2O3/Ni/Ti Composites Enhanced by Intermetallic Phases

In this study, ceramic–metal composites in the Al₂O₃/Ti/Ni system were fabricated using the slip casting method. Two series of composites with 15 vol.% metal content and different solid phase contents were obtained and examined. A proper fabrication process allows obtaining composites enhanced by intermetallic phases. The microstructure of the base powders, slurries, and sintered composites was analyzed by scanning electron microscope. Analysis of the sedimentation tendency of slurries was carried out. The phase composition of the sintered samples was examined by X-ray diffraction analysis. A monotonic compression test was used to investigate the mechanical properties of the composites. A fractography investigation was also carried out. The research conducted revealed that the slip casting method allows the obtaining of composites enhanced by intermetallic phases (TiNi, Ni₃Ti). The results show the correlation between solid-phase content, microstructure, and mechanical properties of the composites.     

Initial Processes of Atomic Layer Deposition of Al2O3 on InGaAs: Interface Formation Mechanisms and Impact on Metal-Insulator-Semiconductor Device Performance

Interface-formation processes in atomic layer deposition (ALD) of Al₂O₃ on InGaAs surfaces were investigated using on-line Auger electron spectroscopy. Al₂O₃ ALD was carried out by repeating a cycle of Al(CH₃)₃ (trimethylaluminum, TMA) adsorption and oxidation by H₂O. The first two ALD cycles increased the Al KLL signal, whereas they did not increase the O KLL signal. Al₂O₃ bulk-film growth started from the third cycle. These observations indicated that the Al₂O₃/InGaAs interface was formed by reduction of the surface oxides with TMA. In order to investigate the effect of surface-oxide reduction on metal-insulator-semiconductor (MIS) properties, capacitors and field-effect transistors (FETs) were fabricated by changing the TMA dosage during the interface formation stage. The frequency dispersion of the capacitance-voltage characteristics was reduced by employing a high TMA dosage. The high TMA dosage, however, induced fixed negative charges at the MIS interface and degraded channel mobility.     

Influence of Cr,Mn, Co and Ni Addition on Crystallization Behavior of Al13Fe4 Phase in Al-5Fe Alloys Based on ThermoDynamic Calculations

Alloying is an effective method to refine coarse grains of an Al₁₃Fe₄ phase and strengthen Al-Fe alloys. However, the grain refinement mechanism remains unclear in terms of the thermodynamics. Herein, the influence of M-element, i.e., Cr, Mn, Co and Ni, addition on the activity of Al and Fe atoms, Gibbs free energy of the Al₁₃Fe₄ nucleus in Al-Fe melt and the formation enthalpy of an Al₁₃Fe₄ phase in Al-Fe alloys is systematically investigated using the extended Miedema model, Wilson equation, and first-principle calculations, respectively. The results reveal that the addition of different M elements increases the activity of Fe atoms and reduces the Gibbs free energy of the Al₁₃Fe₄ nucleus in Al-Fe melt, where the incorporation of Ni renders the most obvious effect, followed by Mn, Co, and Cr. Additionally, the formation enthalpy decreases in the following order: Al₇₈(Fe₂₃Cr) > Al₇₈(Fe₂₃Mn) > Al₁₃Fe₄ > Al₇₈(Fe₂₃Ni) > Al₇₈(Fe₂₃Co), where the formation enthalpy of Al₇₈(Fe₂₃Ni) is close to Al₇₈(Fe₂₃Co). Moreover, the presence of Ni promotes the nucleation of the Al₁₃Fe₄ phase in Al-Fe alloys, which reveals the mechanism of grain refinement from a thermodynamics viewpoint.     

Microstructure Evolution Mechanism of Wf/Cu82Al10Fe4Ni4 Composites under Dynamic Compression at Different Temperatures and Strain Rates

W_f/Cu₈₂Al₁₀Fe₄Ni₄ composites were fabricated by the pressure infiltration method. The composites were compressed by means of a split Hopkinson pressure bar (SHPB) with strain rates of 800 and 1600 s⁻¹ at different temperatures. The microstructure of the composites after dynamic compressing was analyzed by transmission electron microscopy (TEM). Observation revealed that there were high-density dislocations, stacking faults, twins, and recrystallization existing in the copper alloy matrix of the composites. High-density dislocations, stacking faults, and twins were generated due to the significant plastic deformation of the copper alloy matrix under dynamic load impact. We also found that the precipitated phase of the matrix played a role in the second phase strengthening; recrystallized microstructures of copper alloy were generated due to dynamic recrystallization of the copper alloy matrix under dynamic compression at high temperatures.     

Sintering Behavior,Thermal Expansion,and Environmental Impacts Accompanying Materials of the Al2O3/ZrO2 System Fabricated via Slip Casting

This work focuses on research on obtaining and characterizing Al₂O₃/ZrO₂ materials formed via slip casting method. The main emphasis in the research was placed on environmental aspects and those related to the practical use of ceramic materials. The goal was to analyze the environmental loads associated with the manufacturing of Al₂O₃/ZrO₂ composites, as well as to determine the coefficient of thermal expansion of the obtained materials, classified as technical ceramics. This parameter is crucial in terms of their practical applications in high-temperature working conditions, e.g., as parts of industrial machines. The study reports on the four series of Al₂O₃/ZrO₂ materials differing in the volume content of ZrO₂. The sintering process was preceded by thermogravimetric measurements. The fabricated and sintered materials were characterized by dilatometric study, scanning electron microscopy, X-ray diffraction, and stereological analysis. Further, life cycle assessment was supplied. Based on dilatometric tests, it was observed that Al₂O₃/ZrO₂ composites show a higher coefficient of thermal expansion than that resulting from the content of individual phases. The results of the life cycle analysis showed that the environmental loads (carbon footprint) resulting from the acquisition and processing of raw materials necessary for the production of sinters from Al₂O₃ and ZrO₂ are comparable to those associated with the production of plastic products such as polypropylene or polyvinyl chloride.     

Organometallic Routes into the Nanorealms of Binary Fe-Si Phases

The Fe-Si binary system provides several iron silicides that have varied and exceptional material properties with applications in the electronic industry. The well known Fe-Si binary silicides are Fe₃Si, Fe₅Si₃, FeSi, α-FeSi₂ and β-FeSi₂. While the iron-rich silicides Fe₃Si and Fe₅Si₃ are known to be room temperature ferromagnets, the stoichiometric FeSi is the only known transition metal Kondo insulator. Furthermore, Fe₅Si₃ has also been demonstrated to exhibit giant magnetoresistance (GMR). The silicon-rich β-FeSi₂ is a direct band gap material usable in light emitting diode (LED) applications. Typically, these silicides are synthesized by traditional solid-state reactions or by ion beam-induced mixing (IBM) of alternating metal and silicon layers. Alternatively, the utilization of organometallic compounds with reactive transition metal (Fe)-carbon bonds has opened various routes for the preparation of these silicides and the silicon-stabilized bcc- and fcc-Fe phases contained in the Fe-Si binary phase diagram. The unique interfacial interactions of carbon with the Fe and Si components have resulted in the preferential formation of nanoscale versions of these materials. This review will discuss such reactions.     

Phase Composition of Al-Si Coating from the Initial State to the Hot-Stamped Condition

The chemical and phase composition of the coating and the coating/substrate interface of an Al-Si-coated 22MnB5 hot stamped steel was investigated by means of SEM-EDS, XRD, micro-XRD and electron diffraction. Moreover, the surface profile was analyzed by XPS and roughness measurements. The XPS measurements showed that the thickness of the Si and Al oxide layers increased from 14 to 76 nm after die-quenching, and that the surface roughness increased as well as a result of volume changes caused by phase transformations. In addition to the FeAl(Si) and Fe₂Al₅ phases and the interdiffusion layer forming complex structures in the coating, electron diffraction confirmed the presence of an Fe₂Al₅ phase, and also revealed very thin layers of Fe₃(Al,Si)C, Fe₂(Al,Si)₅ and Al-bearing rod-shaped particles in the immediate vicinity of the steel interface. Moreover, the scattered nonuniform layer of the Fe₂Al₈Si phase was identified in the outermost layer of the coating. Despite numerous studies devoted to researching the phase composition of the Al-Si coating applied to hot stamped steel, electron diffraction revealed very thin layers and particles on the coating/substrate interface and outermost layer, which have not been analyzed in detail.     

Characterization of Al2O3 Matrix Composites Fabricated via the Slip Casting Method Using NiAl-Al2O3 Composite Powder

This work aimed to characterize Al₂O₃ matrix composites fabricated by the slip casting method using NiAl-Al₂O₃ composite powder as the initial powder. The composite powder, consisting of NiAl + 30 wt.% Al₂O₃, was obtained by mechanical alloying of Al₂O₃, Al, and Ni powders. The composite powder was added to the Al₂O₃ powder to prepare the final powder for the slip casting method. The stained composite samples presented high density. EDX and XRD analyses showed that the sintering process of the samples in an air atmosphere caused the formation of the NiAl₂O₄ spinel phase. Finally, the phase composition of the composites changed from the initial phases of Al₂O₃ and NiAl to Al₂O₃, Ni, and NiAl₂O₄. However, in the area of Ni, fine Al₂O₃ particles remaining from the initial composite powder were visible. It can be concluded that after slip casting, after starting with Al₂O₃ and the composite powder (NiAl-Al₂O₃) and upon sintering in air, ceramic matrix composites with Ni and NiAl₂O₄ phases, complex structures, high-quality sintered samples, and favorable mechanical properties were obtained.     

High-Temperature Chemical Stability of Cr(III) Oxide Refractories in the Presence of Calcium Aluminate Cement

Al₂O₃-CaO-Cr₂O₃ castables are used in various furnaces due to excellent corrosion resistance and sufficient early strength, but toxic Cr(VI) generation during service remains a concern. Here, we investigated the relative reactivity of analogous Cr(III) phases such as Cr₂O₃, (Al_1−xCr_x)₂O₃ and in situ Cr(III) solid solution with the calcium aluminate cement under an oxidizing atmosphere at various temperatures. The aim is to comprehend the relative Cr(VI) generation in the low-cement castables (Al₂O₃-CaO-Cr₂O₃-O₂ system) and achieve an environment-friendly application. The solid-state reactions and Cr(VI) formation were investigated using powder XRD, SEM, and leaching tests. Compared to Cr₂O₃, the stability of (Al_1−xCr_x)₂O₃ against CAC was much higher, which improved gradually with the concentration of Al₂O₃ in (Al_1−xCr_x)₂O₃. The substitution of Cr₂O₃ with (Al_1−xCr_x)₂O₃ in the Al₂O₃-CaO-Cr₂O₃ castables could completely inhibit the formation of Cr(VI) compound CaCrO₄ at 500–1100 °C and could drastically suppress Ca₄Al₆CrO₁₆ generation at 900 to 1300 °C. The Cr(VI) reduction amounting up to 98.1% could be achieved by replacing Cr₂O₃ with (Al_1−xCr_x)₂O₃ solid solution. However, in situ stabilized Cr(III) phases as a mixture of (Al_1−xCr_x)₂O₃ and Ca(Al_12−xCr_x)O₁₉ solid solution hardly reveal any reoxidation. Moreover, the CA₆ was much more stable than CA and CA₂, and it did not participate in any chemical reaction with (Al_1−xCr_x)₂O₃ solid solution.     

Pulse Plasma Sintering of NiAl-Al2O3 Composite Powder Produced by Mechanical Alloying with Contribution of Nanometric Al2O3 Powder

NiAl-Al₂O₃ composites, fabricated from the prepared composite powders by mechanical alloying and then consolidated by pulse plasma sintering, were presented. The use of nanometric alumina powder for reinforcement of a synthetized intermetallic matrix was the innovative concept of this work. Moreover, this is the first reported attempt to use the Pulse Plasma Sintering (PPS) method to consolidate composite powder with the contribution of nanometric alumina powder. The composite powders consisting of the intermetallic phase NiAl and Al₂O₃ were prepared by mechanical alloying from powder mixtures containing Ni-50at.%Al with the contribution of 10 wt.% or 20 wt.% nanometric aluminum oxide. A nanocrystalline NiAl matrix was formed, with uniformly distributed Al₂O₃ inclusions as reinforcement. The PPS method successfully consolidated NiAl-Al₂O₃ composite powders with limited grain growth in the NiAl matrix. The appropriate sintering temperature for composite powder was selected based on analysis of the grain growth and hardness of Al₂O₃ subjected to PPS consolidation at various temperatures. As a result of these tests, sintering of the NiAl-Al₂O₃ powders was carried out at temperatures of 1200 °C, 1300 °C, and 1400 °C. The microstructure and properties of the initial powders, composite powders, and consolidated bulk composite materials were characterized by SEM, EDS, XRD, density, and hardness measurements. The hardness of the ultrafine-grained NiAl-Al₂O₃ composites obtained via PPS depends on the Al₂O₃ content in the composite, as well as the sintering temperature applied. The highest values of the hardness of the composites were obtained after sintering at the lowest temperature (1200 °C), reaching 7.2 ± 0.29 GPa and 8.4 ± 0.07 GPa for 10 wt.% Al₂O₃ and 20 wt.% Al₂O₃, respectively, and exceeding the hardness values reported in the literature. From a technological point of view, the possibility to use sintering temperatures as low as 1200 °C is crucial for the production of fully dense, ultrafine-grained composites with high hardness.     

Direct Electrochemistry and Electrocatalysis of Horseradish Peroxidase Immobilized in a DNA/Chitosan-Fe3O4 Magnetic Nanoparticle Bio-Complex Film

A DNA/chitosan-Fe₃O₄ magnetic nanoparticle bio-complex film was constructed for the immobilization of horseradish peroxidase (HRP) on a glassy carbon electrode. HRP was simply mixed with DNA, chitosan and Fe₃O₄ nanoparticles, and then applied to the electrode surface to form an enzyme-incorporated polyion complex film. Scanning electron microscopy (SEM) was used to study the surface features of DNA/chitosan/Fe₃O₄/HRP layer. The results of electrochemical impedance spectroscopy (EIS) show that Fe₃O₄ and enzyme were successfully immobilized on the electrode surface by the DNA/chitosan bio-polyion complex membrane. Direct electron transfer (DET) and bioelectrocatalysis of HRP in the DNA/chitosan/Fe₃O₄ film were investigated by cyclic voltammetry (CV) and constant potential amperometry. The HRP-immobilized electrode was found to undergo DET and exhibited a fast electron transfer rate constant of 3.7 s⁻¹. The CV results showed that the modified electrode gave rise to well-defined peaks in phosphate buffer, corresponding to the electrochemical redox reaction between HRP(Fe^(III)) and HRP(Fe^(II)). The obtained electrode also displayed an electrocatalytic reduction behavior towards H₂O₂. The resulting DNA/chitosan/Fe₃O₄/HRP/glassy carbon electrode (GCE) shows a high sensitivity (20.8 A·cm⁻²·M⁻¹) toward H₂O₂. A linear response to H₂O₂ measurement was obtained over the range from 2 μM to 100 μM (R² = 0.99) and an amperometric detection limit of 1 μM (S/N = 3). The apparent Michaelis-Menten constant of HRP immobilized on the electrode was 0.28 mM. Furthermore, the electrode exhibits both good operational stability and storage stability.     

Enhanced Cyclability of Cr8O21 Cathode for PEO-Based All-Solid-State Lithium-Ion Batteries by Atomic Layer Deposition of Al2O3

Cr₈O₂₁ can be used as the cathode material in all-solid-state batteries with high energy density due to its high reversible specific capacity and high potential plateau. However, the strong oxidation of Cr₈O₂₁ leads to poor compatibility with polymer-based solid electrolytes. Herein, to improve the cycle performance of the battery, Al₂O₃ atomic layer deposition (ALD) coating is applied on Cr₈O₂₁ cathodes to modify the interface between the electrode and the electrolyte. X-ray photoelectron spectroscopy, scanning electron microscope, transmission electron microscope, and Fourier transform infrared spectroscopy, etc., are used to estimate the morphology of the ALD coating and the interface reaction mechanism. The electrochemical properties of the Cr₈O₂₁ cathodes are investigated. The results show that the uniform and dense Al₂O₃ layer not only prevents the polyethylene oxide from oxidization but also enhances the lithium-ion transport. The 12-ALD-cycle-coated electrode with approximately 4 nm Al₂O₃ layer displays the optimal cycling performance, which delivers a high capacity of 260 mAh g⁻¹ for the 125th cycle at 0.1C with a discharge-specific energy of 630 Wh kg⁻¹.     

Al2O3/ZrO2/Y3Al5O12 Composites: A High-Temperature Mechanical Characterization

An Al₂O₃/5 vol%·ZrO₂/5 vol%·Y₃Al₅O₁₂ (YAG) tri-phase composite was manufactured by surface modification of an alumina powder with inorganic precursors of the second phases. The bulk materials were produced by die-pressing and pressureless sintering at 1500 °C, obtaining fully dense, homogenous samples, with ultra-fine ZrO₂ and YAG grains dispersed in a sub-micronic alumina matrix. The high temperature mechanical properties were investigated by four-point bending tests up to 1500 °C, and the grain size stability was assessed by observing the microstructural evolution of the samples heat treated up to 1700 °C. Dynamic indentation measures were performed on as-sintered and heat-treated Al₂O₃/ZrO₂/YAG samples in order to evaluate the micro-hardness and elastic modulus as a function of re-heating temperature. The high temperature bending tests highlighted a transition from brittle to plastic behavior comprised between 1350 and 1400 °C and a considerable flexural strength reduction at temperatures higher than 1400 °C; moreover, the microstructural investigations carried out on the re-heated samples showed a very limited grain growth up to 1650 °C.     

The Effect of Temperature and Sputtered Particles on the Wettability of Al/Al2O3

Two kinds of Al₂O₃ ceramic samples with and without Al film deposited were designed respectively. The influences of temperature and high kinetic energy sputtering particles on the wettability and interface strength of Al/Al₂O₃ were studied by comparing the wetting behavior of molten aluminum on two samples. The results show that molten aluminum does not wet the Al₂O₃ sample without Al film deposited at 700 °C, the contact angle is 165°, and the interfacial shear strength is 28 MPa. With the increase of temperature, the contact angle decreases continuously, and the interface shear strength gradually increases. The fracture of the brazed joint is transferred from the interface to the brazing seam. In comparison, the sample deposited with Al film is wetted by molten aluminum at 700 °C, and the contact angle is only 12°. The interface shear strength is about 120 MPa and is less affected by temperature. The shear fracture of the joint occurs in the brazed seam of Al metal. Therefore, the high energy generated by either the temperature increase or the particle sputtering enable the Al atoms to overcome the energy barrier to form Al–O bonds with the O atoms on the Al₂O₃ ceramic surface, thereby improving the wettability of Al/Al₂O₃.     

Behaviour of Microwave-Heated Al4SiC4 at 2.45 GHz

The ongoing development of high-temperature processes with the use of microwaves requires new microwave absorbers that are useful at these temperatures. In this study, we propose Al₄SiC₄ powders as important and efficient microwave absorbers. We investigated both the behavioural microwave heating and electrical permittivity characteristics of Al₄SiC₄ powders with various particle sizes at 2.45 GHz. The TE₁₀₃ single-mode cavity indicated that Al₄SiC₄ powder samples yielded different heating behaviours and dielectric constants for each particle size compared with SiC. By microwave heating ∅50 mm × 5 mm disks of Al₄SiC₄ and SiC, we demonstrate that for specific sizes, Al₄SiC₄ can be heated at a higher temperature than SiC. Finally, the results of the two-dimensional two-colour thermometer show that an energy concentration appears at the interface of the microwave-heated Al₄SiC₄. These phenomena, which are inconsistent in individual physical property values, can be explained without contradicting microwave heating physics.     

Al2O3-Cu-Ni Composites Manufactured via Uniaxial Pressing: Microstructure,Magnetic, and Mechanical Properties

This study’s main goal was to obtain and characterize Al₂O₃-Cu-Ni composites with different metallic phase content. The study analyzed the three series of samples differing in the metallic phase 5, 10, 15 vol.% volume contents. An identical volume share of the metallic components in the metallic phase was used. Ceramic–metal composites were formed using uniaxial pressing and sintered at a temperature of 1400 °C. The microstructural investigation of the Al₂O₃-Cu-Ni composite and its properties involved scanning electron microscopes observations and X-ray diffraction. The size of the metallic phase in the ceramic matrix was performed using a stereological analysis. Microhardness analysis with fracture toughness measures was applied to estimate the mechanical properties of the prepared materials. Additionally, magnetic measurements were carried out, and the saturation magnetization was determined on the obtained magnetic hysteresis loops. The prepared samples, regardless of the content of the metallic phase in each series, were characterized by a density exceeding 95% of the theoretical density. The magnetic measurements exhibited that the fabricated composites had ferromagnetic properties due to nickel and nickel-rich phases. The hardness of the samples containing 5, 10, 15 vol.% metallic phases decreased with an increase in the metallic phase content, equal to 17.60 ± 0.96 GPa, 15.40 ± 0.81 GPa, 12.6 ± 0.36 GPa, respectively.     

Chemical and Structural Changes by Gold Addition Using Recharge Method in NiW/Al2O3-CeO2-TiO2 Nanomaterials

NiWAu trimetallic nanoparticles (NPs) on the surface of support Al₂O₃-CeO₂-TiO₂ were synthesized by a three-step synthetic method in which Au NPs were incorporated into presynthesized NiW/Al₂O₃-CeO₂-TiO₂. The recharge method, also known as the redox method, was used to add 2.5 wt% gold. The Al₂O₃-CeO₂-TiO₂ support was made by a sol–gel method with two different compositions, and then two metals were simultaneously loaded (5 wt% nickel and 2.5 wt% tungsten) by two different methods, incipient wet impregnation and ultrasound impregnation method. In this paper, we study the effect of Au addition using the recharge method on NiW nanomaterials supported on mixed oxides on the physicochemical properties of synthesized nanomaterials. The prepared nanomaterials were characterized by scanning electron microscopy, BET specific surface area, X-ray diffraction, diffuse reflectance spectroscopy in the UV–visible range and temperature-programmed desorption of hydrogen. The experimental results showed that after loading of gold, the dispersion was higher (46% and 50%) with the trimetallic nanomaterials synthesized by incipient wet impregnation plus recharge method than with impregnation plus ultrasound recharge method, indicating a greater number of active trimetallic (NiWAu) sites in these materials. Small-sized Au from NiWAu/ACTU1 trimetallic nanostructures was enlarged for NiWAu/ACT1. The strong metal NPs–support interaction shown for the formation of NiAl₂O₄, Ni-W-O and Ni-Au-O species simultaneously present in the surface of trimetallic nanomaterial probably plays an important role in the degree of dispersion of the gold active phase.