Direct-bonded Al/Al2O3 using a transient eutectic liquid phase

Directed bonding with Al and Al₂O₃ was achieved using a transient liquid phase (TLP) method after annealing at the low melting point of Al, which deposited Ni, Cu, Ge, and Si on the Al₂O₃ substrate. Al/Al₂O₃ microstructures were evaluated using a scanning electron microscopy and transmission electron microscopy. A reaction layer was absent at the Al/Al₂O₃ interface, and all deposited metal films dissolved into the Al foil and reacted with Al to form an eutectic liquid phase near the interface to wet and join with the Al₂O₃. Al₉Fe₂ and Al₃Fe intermetallic compounds were formed in the Al substrate because of Fe precipitation, which is an impurity of Al foil, and the reaction with Al at the grain boundaries of Al. The bonding area percentage, shear strength, and thermal conductivity for Al and Al₂O₃ were assessed using scanning acoustic tomography (SAT), the ISO 13 124 shear strength test, and the laser flash method, respectively. The Al/Al₂O₃ specimen deposited with the Ni film had the highest shear strength (33.74 MPa), thermal conductivity (42.3 W/mK), and bonding area percentage (96.78%). The Al/Al₂O₃ specimens deposited with Ge and Si exhibited relatively poor bonding because of the oxidation of Ge and Si at the surface of Al₂O₃ before bonding with Al.     

Fabrication and characterization of aluminum nitride thick film coated on aluminum substrate for heat dissipation

For effective heat dissipation in high-power LED applications, aluminum nitride (AlN) thick films as thermally conductive dielectric layers were developed, which were deposited on an Al substrate by aerosol deposition (AD). The aerosol-deposited AlN thick films on Al substrates have advantages over conventional polymer-based dielectric substrates or ceramic substrate mounted heatsink systems including an epoxy adhesive, such as excellent heat dissipation capacity and low thermal resistance. AD is an effective method to fabricate high-quality AlN thick film without the Al₂O₃ phase because the film is formed at room temperature. Highly dense and well-adhered, pure AlN thick films with thicknesses up to 30 µm were deposited on an Al substrate. AlN-Al₂O₃ and AlN-polyvinylidene fluoride (PVDF) composite films were also deposited on an Al substrate in order to investigate the effect of Al₂O₃ and polymer on the microstructure and thermal properties. Among the films, pure AlN thick film exhibited the highest dielectric strength, the highest thermal conductivity, and the lowest thermal resistance. Therefore, it can be expected that the aerosol-deposited AlN thick film on Al substrate could be used as a powerful heatsink.     

Yb2Si2O7 Environmental barrier coatings with reduced bond coat oxidation rates via chemical modifications for long life

Spallation of environmental barrier coating (EBC) induced by thermally grown oxide (TGO) resulting from steam oxidation is a key EBC failure mode. A logical approach to improve EBC life, therefore, is to reduce TGO growth rates. A study was undertaken to investigate whether TGO growth rates can be reduced by adding modifier oxides. It was based on a hypothesis that modifier oxides dissolve in SiO₂ TGO and modify the SiO₂ structure, making the TGO less permeable to oxidants. Using a current state-of-the-art EBC (Si/Yb₂Si₂O₇) as the baseline, the Yb₂Si₂O₇ layer was modified by adding Al₂O₃ or Al₂O₃-containing oxide compounds, such as mullite and YAG (Y₃Al₅O₁₂), and TiO₂. EBCs were processed using air plasma spraying. Steam oxidation tests and post-oxidation test oxidation kinetics, chemistry, microstructure, and phase analysis were used to test the hypothesis. The best modified EBC reduced the TGO thickness by ~87% compared with that of the baseline EBC in 90% H₂O + 10% O₂ at 1316°C under thermal cycling. Correlations between oxidation kinetics, chemistry, and microstructure of EBC and TGO were used to explain the effect of modifier oxides on reducing TGO growth rates.     

The effect of Al content on the wettability between liquid iron and MgOAl2O3 binary substrate

In the present study, the wettability between liquid iron with two different Al contents and MgOAl₂O₃ binary substrates was studied in reducing atmosphere. The contact angles between liquid iron with 18?ppm Al and MgO, MgO·Al₂O₃, Al₂O₃ were 133.5°, 113.7°, 126.9° respectively. With the variation of the substrate composition, the contact angles for the intermediate binary phases of the three components (MgO, MgO·Al₂O₃, Al₂O₃) obeyed the Cassie theory. In the experiment using iron with 370?ppm Al, all the contact angles were higher than that using low Al-containing iron. The surface of the iron drop was covered with an oxide layer, which mainly consisted of many small particles. With the variation of the substrate gradually from MgO to Al₂O₃, the composition of the oxide layer changed from MgO·Al₂O₃ to CaOAl₂O₃. The formation of the oxide layer prevented the spreading of liquid iron, leading to the increase of the contact angle.     

Plasma resistance of quartz with a glass coating layer by aerosol deposition

ABSTRACT

To improve the plasma resistance behaviour, glass frits of SiO₂–Al₂O₃–Y₂O₃ with various powder sizes were coated onto quartz substrates by the aerosol deposition (AD) method. The thickness and microstructure of the coating layers were observed using a surface profiler and scanning electron microscopy. Plasma resistance was measured via the quartz substrate, after exposure to an inductively coupled plasma etcher. The coating layers were densely formed on the quartz substrates without additional heat treatment, and the layer thickness changed for the glass frit size distribution and AD process conditions. The SiO₂–Al₂O₃–Y₂O₃ glass coating layer showed a higher plasma resistance than quartz. Furthermore, the AD coating layer was evenly etched after plasma exposure. This study improves the lifetime of plasma chamber components in the semiconductor industry.     

Effect of the thickness of nickel film interlayer on direct-bonded aluminum/alumina as substrate in high-power devices

Aluminum (Al) was successfully bonded with alumina (Al₂O₃) using Ni films of different thicknesses (3, 6, 12 μm) through electroplating and electroless plating processes after annealing at the relatively low melting point of Al. The microstructure, bonding area percentage, shear strength, and thermal conductivity of Al/Al₂O₃ joints were evaluated using scanning electron microscopy, scanning acoustic tomography (SAT), the ISO 13124 test, and the laser flash method respectively. No reaction layer was found at the interface of the Al/Al₂O₃ joint, and the Ni film diffused completely into Al to form an intermetallic compound, Al₃Ni, in the Al foil. The amount and size of the Al₃Ni phase in the Al foil increased gradually with the thickness of the Ni film. The samples with Ni deposited via electroplating had a higher shear stress and bonding area than the samples with Ni deposited via electroless plating. The Al/Al₂O₃ specimen with a 3-μm-thick Ni film interlayer deposited using electroplating had the highest shear strength (50.6 MPa), thermal conductivity (39.45 W/mK), and bonding area percentage (~99.97%); therefore, specimens produced under these conditions were considered suitable for use as a substrate in high-power devices.     

Microstructure and mechanical properties of Al2O3 ceramic and TiAl alloy joints brazed with Ag–Cu–Ti filler metal

Al₂O₃ ceramic was reliably joined to TiAl alloy by active brazing using Ag–Cu–Ti filler metal, and the effects of brazing temperature, holding time, and Ti content on the microstructure and mechanical properties of Al₂O₃/TiAl joints were investigated. The typical interfacial microstructure of joints brazed at 880 °C for 10 min was Al₂O₃/Ti₃(Cu,Al)₃O/Ag(s.s)+AlCu₂Ti+Ti(Cu,Al)+Cu(s.s)/AlCu₂Ti+AlCuTi/TiAl alloy. With increasing brazing temperature and time, the thickness of the Ti₃(Cu,Al)₃O reaction layer increased, and the blocky AlCu₂Ti compounds aggregated and grew gradually. The Ti dissolved from the TiAl substrate was sufficient to react with Al₂O₃ ceramic to form a thin Ti₃(Cu,Al)₃O layer when Ag–Cu eutectic alloy was used, but the dissolution of TiAl alloy was inhibited with an increase in Ti content in the brazing filler. Ti and Al dissolved from the TiAl alloy had a strong influence on the microstructural evolution of the Al₂O₃/TiAl joints, and the mechanism is discussed. The maximum shear strength was 94 MPa when the joints were brazed with commercial Ag–Cu–Ti filler metal, while it reached 102 MPa for the joint brazed with Ag–Cu+2 wt% TiH₂ at 880 °C for 10 min. Fractures propagated primarily in the Al₂O₃ substrate and partially along the reaction layer.     

An evaluation of plasma-sprayed coatings based on Al2O3 and Al2O3–13 wt.% TiO2 with bond coat on pure titanium substrate

In this study, the effects of bond coat on the properties of Al₂O₃ and Al₂O₃–13 wt.% TiO₂ coatings, which is plasma sprayed onto a commercial pure titanium substrate with and without Ni–5 wt.% Al (METCO 450 NS) as bond coating layer were investigated in terms of microhardness, bonding strength and surface roughness. Optical and scanning electron microscopy (SEM) examinations revealed that there is a uniform coating layer with no spalling and delamination. However, there is a little amount of porosity. The results indicated that the application of bond coat layer in the plasma spraying of Al₂O₃ and Al₂O₃–13 wt.% TiO₂ on pure titanium substrate has increased the hardness and bonding strength of coatings. While the adhesive bonding is dominant without bond coat, the cohesive bonding is dominant with the application of the bond coating layer. It has been observed that percentage of cohesion strength was about three times higher than that of adhesion strength.     

Air plasma-sprayed Y2O3 coatings for Al2O3/Al2O3 ceramic matrix composites

Al₂O₃/Al₂O₃ ceramic matrix composites (CMC) are candidate materials for hot-gas leading components of gas turbines. Since Al₂O₃/Al₂O₃ CMC are prone to hot-corrosion in combustion environments, the development of environmental barrier coatings (EBC) is mandatory. Owing to its favorable chemical stability and thermal properties, Y₂O₃ is considered a candidate EBC material for Al₂O₃/Al₂O₃ CMC. Up to 1 mm thick Y₂O₃ coatings were deposited by means of air plasma spraying (APS) on Al₂O₃/Al₂O₃ CMC with a reaction-bonded Al₂O₃ bond-coat (RBAO). APS Y₂O₃ coatings exhibit a good adherence in the as-deposited state as well as upon isothermal annealing up to 1400 °C. Moreover, furnace cyclic testing performed at 1200 °C revealed an excellent durability. This is explained by the formation of a continuous, approximately 1 μm thick reaction zone at the APS Y₂O₃/RBAO interface. The reaction zone between Y₂O₃ and Al₂O₃ comprises three layers of thermodynamically stable yttrium-aluminates exhibiting strong bonding, respectively.     

Corrosion resistance of AlN and Fe3Al reinforced Fe-based plasma cladding layer in 3.5 wt% NaCl solution

Fe-based cladding layers were prepared via the plasma cladding method using nitrogen as protective and reactant gas. The effects of Al on the phase structure, morphology, composition, and corrosion resistance of the cladding layers were investigated. The based cladding layer consisted of α-Fe, Cr, and small amounts of CrN and Fe_xN, whereas Fe₃Al, Cr₅Al₈ and AlN occurred in the cladding layer with Al. Many AlN particles less than 4 μm in diameter were uniformly distributed in the cladding layer. The nitrides in the cladding layer could accelerate the formation of a passive film and increase the corrosion resistance of the cladding layer. A compact and stable passive film composed of Al₂O₃, Cr₂O₃, α-FeOOH, and Fe₃O₄ formed on the surface of the cladding layer with Al, which is beneficial in protecting the substrate and significantly improving the cladding layer's corrosion resistance.     

Microstructure evolution of Al2O3/Al2O3 joint brazed with Ag-Cu-Ti + B + TiH2 composite filler

Al₂O₃/Al₂O₃ joint was achieved using Ag-Cu-Ti + B + TiH₂ composite fillers at 900 °C for 10 min. The evolution mechanism of interface during brazing was discussed. Effects of Ti and B atoms content on microstructure of joints were investigated. Results show that a continuous and compact reaction layer Ti₃(Cu,Al)₃O forms at Al₂O₃/brazing alloy interface. Ti(Cu,Al) precipitates near Ti₃(Cu,Al)₃O layer. In situ synthesized TiB whiskers evenly distribute in Ag and Cu based solid solution. The higher content of B powders in composite fillers increases TiB whiskers content, but decreases the thickness of Ti₃(Cu,Al)₃O layer, while the higher TiH₂ powders content thickens Ti₃(Cu,Al)₃O layer. Ag and Cu based solid solutions become uniform and fine with the increasing of TiB whiskers content. Ti(Cu,Al) intermetallics content increase and they gradually distribute from Al₂O₃ side to the central of brazing alloy, but the content of Cu based solid solution decreases when the TiH₂ content increases.     

Texture development in Fe-doped alumina ceramics via templated grain growth and their application to carbon nanotube growth

Fe-doped alumina (Fe-Al₂O₃) materials with a controlled microstructure could be designed for some special uses such as a substrate for carbon nanotube growth. In this study, Fe-doped Al₂O₃ ceramics with varying degrees of texture were prepared via Templated Grain Growth method and utilized for carbon nanotube synthesis by Catalytic Chemical Vapor Deposition in order to investigate how α-Al₂O₃ crystal orientation affects carbon nanotube growth in polycrystalline ceramics. The degree of texture increased with the Fe content in the presence of liquid phase. Three kinds of carbon filaments (few-wall carbon nanotubes bundles, individual multi-wall nanotubes and carbon nanofibres) were observed over Fe-doped Al₂O₃ ceramics with varying degrees of texture depending on the surface roughness, crystallographic orientation and the size of the catalyst nanoparticles. While well-textured substrates with a rough surface led to a small amount of randomly oriented carbon nanotube bundles, perpendicularly oriented individual multi-wall nanotubes were obtained over relatively smooth single crystal α-Al₂O₃ platelet surfaces (basal planes) which remained in the matrix without growing.     

Understanding the protective role of a gradient titanium oxide ceramic layer on Ti6Al4V against corrosion via analyses of Mott-Schottky curve and electron work function (EWF)

Thermal oxidation (TO) process was employed to generate a gradient titanium oxide ceramic layer for improving corrosion performance and service safety of Ti6Al4V alloy. The semiconductor characteristic of the TO layer was evaluated in CO₂-saturated simulated oilfield brine. The generated TO layer with a thickness of about 20 μm was dense and continuous without cracks or spalling characteristics. The TO layer mainly comprised of an oxide ceramic layer (rutile TiO₂ ceramic phase, minor anatase one, and Al₂O₃) and an oxygen diffusion layer. The conducted electrochemical analysis suggested that the corrosion resistance of Ti6Al4V alloy was improved using TO surface strengthening process. It was demonstrated that the TO layer with semiconductor characteristics showed a transition from n-type (donor) to p-type (acceptor) with the increasing applied electric potential. The electron work function of the TO layer was higher than that of Ti6Al4V alloy with a naturally formed passive film. The improvement in corrosion properties was attributed to the excellent chemical stability and semiconductor properties of the metal oxide ceramic phases (TiO₂, Al₂O₃) in the TO layer.     

Mechanical performances of AlN/Al metallized ceramic substrates fabricated by transient liquid phase bonding and pre-oxidation treatment

For the miniaturization of high-power electronic components, AlN/Al is a promising metallized ceramic substrate due to its superior mechanical and thermal performances. Numerous bonding processes have been proposed for fabricating the metallized ceramic substrate. Unfortunately, the influences of various bonding techniques on the mechanical performance of AlN/Al metallized ceramic substrate remain undetermined to date. The objective of this study was thus to investigate the effects of the transient liquid phase (TLP) technique and pre-oxidation treatment on the bonding, microstructure, and mechanical strength of the AlN/Al metallized ceramic substrate.The results indicated that the three-layered AlN/Al/AlN specimen could be effectively bonded by the TLP process and pre-oxidation treatment. However, the bending strengths of the specimens fabricated by the two techniques were obviously divergent. The bending strength of raw AlN substrate was 333 MPa. In contrast, the bending strengths of the three-layered specimens with AlN substrates pre-oxidized at 1050 °C, 1150 °C, and 1250 °C were 292 MPa, 250 MPa, and 224 MPa, respectively. Raising the pre-oxidation temperature of the AlN substrate from 1050 °C to 1250 °C obviously increased the thickness of the Al₂O₃ layer and deteriorated the bending strength, for the fracture propagated along the Al₂O₃ layer and the Al₂O₃/AlN interface. For the TLP bonding, the Cu film deposited on the AlN substrate contributed to the generation of Al–Cu transient liquid and to bonding. The bending strength of the three-layered specimens fabricated by TLP at 650 °C was 417 MPa, which was 25% and 43% better than those of the raw AlN substrate and the three-layered specimens prepared by the pre-oxidation treatment, respectively.     

Colloidal co-assembly of dual-phased ceramic/metal particles toward lightweight,hierarchically structured,and mechanically robust alumina foam

Ceramic foams constructed by aqueous-based foam templating have demonstrated great potential in industrial and research applications. However, a multiple-phased suspension with inherently improved complexity inevitably leads to a severe deterioration of foam stability. Herein, we proposed a colloidal co-assembly strategy that introduces Al–Al₂O₃ dual-phased particles for constructing ultralight yet mechanically robust cellular ceramics. Owing to the Al₂O₃ oxidation layer on Al particles, both of Al and Al₂O₃ suspensions demonstrated similar zeta potential and rheological properties, enabling a stable foam structure after colloidal co-assembly. High-temperature oxidation of Al particles contributed to the reinforcement of cell wall and formation of Al₂O₃ whiskers. The calcined products demonstrated a lightweight structure (0.31 g cm⁻³), a robust compressive strength (3.64 MPa) at a porosity level of 88.5%, and a relatively high specific surface area (14.7 m² g⁻¹). The current strategy paves the way for the construction of high-performance ceramic foams for a broad range of applications.     

Effect of physical vapor deposited Al2O3 film on TGO growth in YSZ/CoNiCrAlY coatings

Thermal barrier coatings (TBCs) comprising of yttria stabilized zirconia (YSZ) ceramic top coat and CoNiCrAlY metallic bond coat have been widely used in gas turbines. However, the developed oxides layer in the interface of the top and bond coats during thermal exposure of the TBCs always results in the destruction of the system. In order to restrain the growth of oxides layer and improve the thermal shock resistance of TBCs, a thin Al₂O₃ film was pre-deposited on CoNiCrAlY bond coat by physical vapor deposition (PVD) technology. After thermal exposure, morphologies and phase compositions of the thermal growth oxides (TGO) layer in the conventional and pre-deposited Al₂O₃ film TBCs were examined by scanning electron microscopy (SEM) equipped with energy dispersive spectrometer (EDS). The residual stresses in the coatings were analyzed using micro-Raman spectroscopy (LabRam-1B). It was found that TGO layer formed in the conventional TBCs was mainly composed of Al₂O₃, (Cr,Al)₂O₃ + (Co,Ni)(Cr,Al)₂O₄ + NiO (CSN), and (Cr,Al)₂O₃ + (Co,Ni)(Cr,Al)₂O₄ (CS), while in the treated TBCs, the formed TGO layer appeared more uniform and compact. The CSN and CS clusters, which are normally considered as a weakness for TBCs, were greatly limited. The residual stresses in the TBCs after thermal shock were also reduced by the deposition of Al₂O₃ film.     

Preparation and characterization of NiO/MgO/Al2O3 supported CoPcS catalyst and its application to mercaptan oxidation

MgO/Al₂O₃ and NiO/MgO/Al₂O₃ solid bases were prepared by mixing method. The samples were characterized by X-ray diffraction (XRD), CO₂ temperature-programmed desorption (CO₂-TPD) and surface area measurements. After supported sulfonated cobalt phthalocyanine (CoPcS) the catalytic performance of these catalysts was evaluated in the mercaptan oxidation reaction. The effect of Mg/Al mole ratios on activity, crystal structure, basicity and stability in air was discussed. And the mechanism of the effect of NiO was identified. Results show that the base amount of MgO/Al₂O₃ increases with increasing Mg/Al mole ratio and catalyst with high Mg/Al mole ratio has a higher initial activity. NiO/MgO/Al₂O₃–CoPcS shows a higher initial activity and a much longer lifetime than MgO/Al₂O₃–CoPcS. When nickel oxide is doped into the MgO/Al₂O₃ support more crystal defects are generated, which increases the amount and types of basic sites.     

Al2O3–cyanate ester hybrid thick films through aerosol deposition and resin infiltration

Al₂O₃–cyanate ester hybrid thick films had high Al₂O₃ contents over 75 vol.% were fabricated as 3D integrated substrates. The Al₂O₃–cyanate ester hybrid thick films were completed by resin infiltration of the cyanate ester into the porous Al₂O₃ thick films deposited by aerosol deposition (AD). Al₂O₃ particles were packed as high-density layers in the porous Al₂O₃ thick films by controlling the carrier gas flow rate using AD at room temperature. As dielectric substrate materials, the Al₂O₃–cyanate ester hybrid thick films had dielectric constant of 7.6 and quality (Q) factor of 390, and both were nearly independent of the measuring frequency.     

Preparation of a thick NiAl/Al2O3 coating by embedding method and its corrosion resistance under supercritical water environment

One of the critical issues in the application of supercritical water oxidation technology is to improve the corrosion resistance of reactor materials. Use of Al₂O₃ coating is one of the most promising methods to address this issue. In this study, thick NiAl/Al₂O₃ coatings on Inconel 625 substrates were prepared by a consecutive pack embedding and in-situ thermal oxidation process. The effect of aluminizing and oxidation temperature on phase structure and coating thickness is studied. Results show the diffusion of Al from the exterior to the interior of the alloy matrix to form intermetallic compounds between Al and metal elements in the matrix (Ni, Cr, Mo, etc.). Moreover, the coating thickness can reach above 300 μm at the aluminizing temperature of 950 °C. Increasing the aluminizing temperature above 950 °C will not increase the coating thickness further. After high temperature oxidation subsequently, only phases of NiAl and Al₂O₃ were detected. The formation of Al₂O₃ layer can be ascribed to the surface oxidization of Al. And the NiAl between the alloy substrate and Al₂O₃ coating provides an interfacial layer that can alleviate the crack or exfoliation of ceramic coating due to the mismatching of thermal expand coefficient. The thick NiAl/Al₂O₃ coatings prepared by aluminizing 950 °C and oxidizing at 1100 °C exhibit satisfied corrosion resistance after supercritical water test. This work would provide a significant method to develop advanced ceramics coating for the corrosion resistance of alloys.     

Preparation and formation mechanism of Al-Si/Al2O3 core-shell structured particles fabricated via steam corrosion

In this study, Al-Si/Al₂O₃ core-shell structured particles were fabricated via pressurized steam corrosion for 1 h followed by heating for 3 h at 1100 °C. After steam corrosion, a layer composed of disordered crystals covered the surfaces of the Al-Si alloy particles. After heating, Al-Si/Al₂O₃ core-shell structured particles with complete shells were prepared. The thickness of the shell was approximately 2 μm, and it enclosed the Al-Si alloy core. The shell exhibited excellent thermal stability because, even at 1100 °C, the mass gain ratio of the encapsulated particle was less than 0.5%. Scalloped patterns of alumina were formed by the oxidation of Al, which was inlaid through and upon the alumina shell. The shell formation mechanism suggested that the α-Al₂O₃ shell resulted from the combination of the decomposition of surface Al(OH)₃ crystals and the oxidation of Al from the core.