Mechano-thermal treatment of TiO<Subscript>2</Subscript>-Al powder mixture to prepare TiAl/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composite

In this research, a composite comprising an intermetallic matrix and dispersed Al₂O₃ particles was processed. A mixture of TiO₂ and Al was mechanically activated in the presence of a process control agent and/or without it, in a high-energy planetary ball mill. As a subsequent process, the sample was sintered at various temperatures. The phase composition and morphology of the samples were evaluated by XRD and SEM techniques, respectively. The thermal behavior of the samples milled for 8 h with PVA and/or without it, were also assessed by the DTA technique and compared with one another. The DTA results revealed that addition of PVA shifted the aluminothermic reduction of TiO₂ to higher temperatures; therefore, final composite phases were developed at higher temperatures. The results also showed that addition of PVA during milling caused the final microstructure to coarsen. The XRD pattern of the sample sintered at 700 °C exhibits the existence of TiAl, Ti₃Al, and Al₂O₃ phases. In the sample sintered at 850 °C, the remaining Ti₃Al peak was attenuated and completely disappeared at 1000 °C.     

Microstructure and Mechanical Behavior of Microwave Sintered Cu<Subscript>50</Subscript>Ti<Subscript>50</Subscript> Amorphous Alloy Reinforced Al Metal Matrix Composites

In the present work, Al metal matrix composites reinforced with Cu-based (Cu₅₀Ti₅₀) amorphous alloy particles synthesized by ball milling followed by a microwave sintering process were studied. The amorphous powders of Cu₅₀Ti₅₀ produced by ball milling were used to reinforce the aluminum matrix. They were examined by x-ray diffraction (XRD), scanning electron microscopy (SEM), microhardness and compression testing. The analysis of XRD patterns of the samples containing 5 vol.%, 10 vol.% and 15 vol.% Cu₅₀Ti₅₀ indicates the presence of Al and Cu₅₀Ti₅₀ peaks. SEM images of the sintered composites show the uniform distribution of reinforced particles within the matrix. Mechanical properties of the composites were found to increase with an increasing volume fraction of Cu₅₀Ti₅₀ reinforcement particles. The hardness and compressive strength were enhanced to 89 Hv and 449 MPa, respectively, for the Al-15 vol.% Cu₅₀Ti₅₀ composites.     

Preparation and characterization of nanostructured Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-13wt.%TiO<Subscript>2</Subscript> ceramic coatings by plasma spraying

Nanostructured and conventional Al₂O₃-13wt.%TiO₂ ceramic coatings were prepared by plasma spraying with nanostructured agglomerated and conventional powders, respectively. The microstructure and microhardness of the coatings were investigated using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and microhardness measurement. Meanwhile, the friction and wear behaviors were analyzed and compared using a ball-on-disk tribometer. The results show that the conventional coating has lamellar stacking characteristic and has some pores. However, the nanostructured coating shows a bimodal microstructure, which is composed of both fully melted regions and partially melted regions. According to the microstructural difference, the partially melted regions can be divided into liquid-phase sintered regions (a three-dimensional net or skeleton-like structure: Al₂O₃-rich submicron particles embedded in the TiO₂-rich matrix) and solid-phase sintered regions (remained nanoparticles). The microstructural characteristics of the liquid-phase sintered region are formed due to the selective melting of TiO₂ nanoparticles during plasma spraying. On the other hand, the TiO₂ and Al₂O₃ nanoparticles of the solid-phase sintered regions are all unmelted during plasma spraying. Due to the existence of nanostructured microstructures, the nanostructured coating has a higher microhardness, a lower friction coefficient, and a better wear resistance than the conventional coating.     

Microstructure and Thermomechanical Properties of Atmospheric Plasma-Sprayed Yb<Subscript>2</Subscript>O<Subscript>3</Subscript> Coating

In this study, a Yb₂O₃ coating was fabricated by the atmospheric plasma spray technique. The phase composition, microstructure, and thermal stability of the coating were examined. The thermal conductivity and thermal expansion behavior were also investigated. Some of the mechanical properties (elastic modulus, hardness, fracture toughness, and flexural strength) were characterized. The results reveal that the Yb₂O₃ coating is predominantly composed of the cubic Yb₂O₃ phase, and it has a dense lamellar microstructure containing defects. No mass change and exothermic phenomena are observed in the thermogravimetry and differential thermal analysis curves. The high-temperature x-ray diffraction results indicate that no phase transformation occurs from room temperature to 1500 °C, revealing the good phase stability of the Yb₂O₃ coating. The coefficient of thermal expansion of the Yb₂O₃ coating is (7.50-8.67)?×?10^?6 K^?1 in the range of 200-1400 °C. The thermal conductivity is about 1.5 W m^?1 K^?1 at 1200 °C. The Yb₂O₃ coating has excellent mechanical properties and good damage tolerant. The unique combination of these properties implies that the Yb₂O₃ coating might be a promising candidate for T/EBCs applications.     

Effects of cryogenic treatment on the thermal physical properties of Cu<Subscript>76.12</Subscript>Al<Subscript>23.88</Subscript> alloy

The thermal diffusion coefficient,heat capacity,thermal conductivity,and thermal expansion coefficient of Cu76.12Al23.88 alloy before and after cryogenic treatment in the heating temperature range of 25°C to 600°C were measured by thermal constant tester and thermal expansion instrument.The effects of cryogenic treatment on the thermal physical properties of Cu76.12Al23.88 alloy were investigated by comparing the variation of the thermal parameters before and after cryogenic treatment.The results show that the variation trend of the thermal diffusion coefficient,heat capacity,thermal conductivity,and thermal expansion coefficient of Cu76.12Al23.88 alloy after cryogenic treatment was the same as before.The cryogenic treatment can increase the thermal diffusion coefficient,thermal conductivity,and thermal expansion coefficient of Cu76.12Al23.88 alloy and decrease its heat capacity.The maximum difference in the thermal diffusion coefficient between the before and after cryogenic treatment appeared at 400°C.Similarly,thermal conductivity was observed at 200°C.     

Influence of Feedstock Powder Modification by Heat Treatments on the Properties of APS-Sprayed Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-40% TiO<Subscript>2</Subscript> Coatings

The formation and decomposition of aluminum titanate (Al₂TiO₅, tialite) in feedstock powders and coatings of the binary Al₂O₃-TiO₂ system are so far poorly understood. A commercial fused and crushed Al₂O₃-40%TiO₂ powder was selected as the feedstock for the experimental series presented in this paper, as the composition is close to that of Al₂TiO₅. Part of that powder was heat-treated in air at 1150 and 1500 °C in order to modify the phase composition, while not influencing the particle size distribution and processability. The powders were analyzed by thermal analysis, XRD and FESEM including EDS of metallographically prepared cross sections. Only a maximum content of about 45 wt.% Al₂TiO₅ was possible to obtain with the heat treatment at 1500 °C due to inhomogeneous distribution of Al and Ti in the original powder. Coatings were prepared by plasma spraying using a TriplexPro-210 (Oerlikon Metco) with Ar-H₂ and Ar-He plasma gas mixtures at plasma power levels of 41 and 48 kW. Coatings were studied by XRD, SEM including EDS linescans of metallographically prepared cross sections, and microhardness HV1. With the exception of the powder heat-treated at 1500 °C an Al₂TiO₅-Ti₃O₅ (tialite–anosovite) solid solution Al_2?xTi_1+xO₅ instead of Al₂TiO₅ existed in the initial powder and the coatings.     

Microstructure and Thermal Properties of Atmospheric Plasma-Sprayed Yb<Subscript>2</Subscript>Si<Subscript>2</Subscript>O<Subscript>7</Subscript> Coating

In the present work, Yb₂Si₂O₇ powder was synthesized by solid-state reaction using Yb₂O₃ and SiO₂ powders as starting materials. Atmospheric plasma spray technique was applied to fabricate Yb₂Si₂O₇ coating. The phase composition and microstructure of the coating were characterized. The density, open porosity and Vickers hardness of the coating were investigated. Its thermal stability was evaluated by thermogravimetry and differential thermal analysis (TG-DTA). The thermal diffusivity and thermal conductivity of the coating were measured. The results showed that the as-sprayed coating was mainly composed of crystalline Yb₂Si₂O₇ with amorphous phase. The coating had a dense structure containing defects, such as pores, interfaces and microcracks. The TG-DTA results showed that there was almost no mass change from room temperature to 1200 °C, while a sharp exothermic peak appeared at around 1038 °C in DTA curve, which indicated that the amorphous phase crystallized. The thermal conductivity of the coating decreased with rise in temperature up to 600 °C and then followed by an increase at higher temperatures. The minimum value of the thermal conductivity of the Yb₂Si₂O₇ coating was about 0.68 W/(m K).     

Thermal Spray Deposition,Phase Stability and Mechanical Properties of La<Subscript>2</Subscript>Zr<Subscript>2</Subscript>O<Subscript>7</Subscript>/LaAlO<Subscript>3</Subscript> Coatings

This paper deals with the deposition of La₂Zr₂O₇ (LZO) and LaAlO₃ (LAO) mixtures by air plasma spray (APS). The raw material for thermal spray, single phase LZO and LAO in a 70:30 mol.% ratio mixture was prepared from commercial metallic oxides by high-energy ball milling (HEBM) and high-temperature solid-state reaction. The HEBM synthesis route, followed by a spray-drying process, successfully produced spherical agglomerates with adequate size distribution and powder-flow properties for feeding an APS system. The as-sprayed coating consisted mainly of a crystalline LZO matrix and partially crystalline LAO, which resulted from the high cooling rate experienced by the molten particles as they impact the substrate. The coatings were annealed at 1100 °C to promote recrystallization of the LAO phase. The reduced elastic modulus and hardness, measured by nanoindentation, increased from 124.1 to 174.7 GPa and from 11.3 to 14.4 GPa, respectively, after the annealing treatment. These values are higher than those reported for YSZ coatings; however, the fracture toughness (K _IC) of the annealed coating was only 1.04 MPa m^0.5.     

Synthesis and thermal expansion of 4J36/ZrW<Subscript>2</Subscript>O<Subscript>8</Subscript> composites

Gas atomized 4J36 alloy powder was milled for 72 h then mixed with ZrW₂O₈ powder and sintered at 600°C for 4 h under argon atmosphere. 4J36/ZrW₂O₈ composites containing 10 vol.%, 20 vol.%, 30 vol.%, and 40 vol.% ZrW₂O₈ were fabricated, the relative density of which ranged from 70% to 80%. Thermal expansion coefficients of the composites decreased as the amount of ZrW₂O₈ increased, in agreement with the rule of the mixture. The coefficient of thermal expansion of the 4J36/40 vol.%ZrW₂O₈ composite in 25–100°C is 0.55 × 10⁻⁶/°C.     

Alloying Behavior and Properties of FeSiBAlNiCo<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> High Entropy Alloys Fabricated by Mechanical Alloying and Spark Plasma Sintering

In this paper, FeSiBAlNiCo_x (x = 0.2, 0.8) high-entropy alloy (HEA) powders were fabricated by mechanical alloying process, and the powders milled for 140 h were sintered by spark plasma sintering (SPS) technique. The microstructures and properties of as-milled powders and as-sintered samples were investigated. The results reveal that the final milling products (140 h) of both sample powders present the fully amorphous structure. The increased Co contents obviously enhance the glass forming ability and thermal stability of amorphous HEA powders, which are reflected by the shorter formation time of fully amorphous phase and the higher onset crystallization temperature, respectively. According to coercivity, the as-milled FeSiBAlNiCo_x (x = 0.2, 0.8) powders (140 h) are the semi-hard magnetic materials. FeSiBAlNiCo_0.8 HEA powders possess the highest saturation magnetization and largest remanence ratio. The SPS-ed products of both bulk HEAs are composed of body-centered cubic solid solution, and FeSi and FeB intermetallic phases. They possess the high relative density above 97% and excellent microhardness exceeding 1150 HV. The as-sintered bulks undergo the remarkable increase in saturation magnetization compared with the as-milled state. The SPS-ed FeSiBAlNiCo_0.8 HEA exhibits the soft magnetic properties. The electrochemical corrosion test is carried out in 3.5% NaCl solution. The SPS-ed FeSiBAlNiCo_0.2 HEA reveals the better passivity with low passive current density, and the higher pitting resistance with wide passive region.     

Formation of Cr<Subscript>2</Subscript>O<Subscript>3</Subscript> Diffusion Barrier Between Cr-Contained Stainless Steel and Cold-Sprayed Ni Coatings at High Temperature

A novel approach to prepare a coating system containing an in situ grown Cr₂O₃ diffusion barrier between a nickel top layer and 310SS was reported. Cold spraying was employed to deposit Ni(O) interlayer and top nickel coating on the Cr-contained stainless steel substrate. Ni(O) feedstock was prepared by mechanical alloying of pure nickel powders in ambient atmosphere, acting as an oxygen provider. The post-spray annealing was adopted to grow in situ Cr₂O₃ layer between the substrate and nickel coating. The results revealed that the diffusible oxygen can be introduced into nickel powders by mechanical alloying. The oxygen content increases to 3.25 wt.% with the increase of the ball milling duration to 8 h, while Ni(O) powders maintain a single phase of Ni. By annealing the sample in Ar atmosphere at 900 °C, a continuous Cr₂O₃ layer of 1-2 μm thick at the interface between 310SS and cold-sprayed Ni coating is formed. The diffusion barrier effect evaluation by thermal exposure at 750 °C shows that the Cr₂O₃ oxide layer effectively suppresses the outward diffusion of Fe and Cr in the substrate effectively.     

Phase Relations in the System TiO<Subscript>2</Subscript>-V<Subscript>2</Subscript>O<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> under Oxidizing and Reducing Conditions

The target of this work was to investigate the phase development in the catalyst system consisting of TiO₂ (Anatase) and V₂O₅ (Shcherbinaite) under several gas atmospheres. Thus a set of V₂O₅/TiO₂ specimens was prepared by ball milling and exposed to subsequent annealing in air and feed gas in the temperature range from 400 to 700 °C. The XRD-results showed that the initial phases Anatase and Shcherbinaite remain stable for all atmospheres containing oxygen. In the temperature range above 525 °C the formation of a Rutile solid solution (Rutile-ss) containing VO _x species takes place. However, under reducing conditions (lower oxygen partial pressure) the reduction of V₂O₅ to V₂O₃ was found by X-ray diffraction measurements. There is no miscibility up to 1300 °C followed by the formation of V₂TiO₅ (Berdesinskiite). SEM images underline the reduction by monitoring the change in morphology with respect to the V-containing phases. TiO₂ remains without much alteration. The two phases V₂Ti₇O₁₇ and V₂Ti₃O₉ (Schreyerite) as described in mineralogy have not been observed in these experiments. The knowledge of phase relations helps to find the appropriate processing conditions and to understand the aging phenomena of catalysts.     

Thermoelectric Properties of Cu-doped Bi<Subscript>2−x</Subscript>Sb<Subscript>x</Subscript>Te<Subscript>3</Subscript> Prepared by Encapsulated Melting and Hot Pressing

P-type Bi_2?xSb_xTe₃:Cu_m (x = 1.5–1.7 and m = 0.002–0.003) solid solutions were synthesized using encapsulated melting and were consolidated using hot pressing. The effects of Sb substitution and Cu doping on the charge transport and thermoelectric properties were examined. The lattice constants decreased with increasing Sb and Cu contents. As the amount of Sb substitution and Cu doping was increased, the electrical conductivity increased, and the Seebeck coefficient decreased owing to the increase in the carrier concentration. All specimens exhibited degenerate semiconductor characteristics and positive Hall and Seebeck coefficients, indicating p-type conduction. The increased Sb substitution caused a shift in the onset temperature of the intrinsic transition and bipolar conduction to higher temperatures. The electronic thermal conductivity increased with increasing Sb and Cu contents owing to the increase in the carrier concentration, while the lattice thermal conductivity slightly decreased due to alloy scattering. A maximum figure of merit, ZT_max = 1.25, was achieved at 373 K for Bi_0.4Sb_1.6Te₃:Cu_0.003.     

Mechanical Properties of Layered La<Subscript>2</Subscript>Zr<Subscript>2</Subscript>O<Subscript>7</Subscript> Thermal Barrier Coatings

Lanthanum zirconate (La₂Zr₂O₇) has been proposed as a promising thermal barrier coating (TBC) material due to its low thermal conductivity and high stability at high temperatures. In this work, both single and double-ceramic-layer (DCL) TBC systems of La₂Zr₂O₇ and 8 wt.% yttria-stabilized zirconia (8YSZ) were prepared using air plasma spray (APS) technique. The thermomechanical properties and microstructure were investigated. Thermal gradient mechanical fatigue (TGMF) tests were applied to investigate the thermal cycling performance. The results showed that DCL La₂Zr₂O₇ + 8YSZ TBC samples lasted fewer cycles compared with single-layered 8YSZ TBC samples in TGMF tests. This is because DCL La₂Zr₂O₇ TBC samples had higher residual stress during the thermal cycling process, and their fracture toughness was lower than that of 8YSZ. Bond strength test results showed that 8YSZ TBC samples had higher bond strength compared with La₂Zr₂O₇. The erosion rate of La₂Zr₂O₇ TBC samples was higher than that of 8YSZ samples, due to the lower critical erodent velocity and fracture toughness of La₂Zr₂O₇. DCL porous 8YSZ + La₂Zr₂O₇ had a lower erosion rate than other SCL and DCL La₂Zr₂O₇ coatings, suggesting that porous 8YSZ serves as a stress-relief buffer layer.     

Mechanical alloying characteristic and thermal stability of Al<Subscript>78</Subscript>Fe<Subscript>20</Subscript>Zr<Subscript>2</Subscript> amorphous powders

The powders of pure Al, Fe, and Zr for preparing Al₇₈Fe₂₀Zr₂ were subject to a high-energy planetary ball milling. The microstructure evolution of the mixtures at the different intervals of milling was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). It was found that a nearly complete amorphization could be achieved in the mixtures after ball milling for 23 h. Further ball milling led to the crystallization of the amorphous powders. A long time ball milling, e.g., 160 h, led to a complete crystallization of the amorphous powders and the formation of Al₃Zr and Al1₃Fe₄. The crystallization products caused by ball milling are almost the same as that produced by isothermal annealing of the amorphous powders in vacuum at 800 K for 1 h.     

Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiC Composite Prepared by Spark Plasma Sintering Process: Evaluation of Mechanical and Tribological Properties

Al₂O₃-10TiC composites were synthesized by spark plasma sintering (SPS) process. Microstructural and mechanical properties of the composite reveal homogeneous distribution of the fine TiC particles in the matrix. The samples were produced with different sintering temperature, and it shows that the hardness and density gradually increases with increasing sintering temperature. Abrasion wear test result reveals that the composite sintered at 1500 °C shows high abrasion resistance (wt. loss ~ 0.016 g) and the lowest abrasion resistance was observed for the composite sample sintered at 1100 °C (wt. loss ~ 1.459 g). The profilometry surface roughness study shows that sample sintered at 1100 °C shows maximum roughness (R_a = 6.53 µm) compared to the sample sintered at 1500 °C (R_a = 0.66 µm) corroborating the abrasion wear test results.     

Rapid consolidation of nanocrystalline Ti<Subscript>3</Subscript>Al-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites from mechanically synthesized powders by high frequency induction heated sintering

Nano-powders of Ti₃Al and ²Al₂O₃ were synthesized from 3TiO₂ and 5Al powders by high energy ball milling. Nanocrystalline Al₂O₃ reinforced composite was consolidated by high frequency induction heated sintering within 2 minutes from mechanochemically synthesized powders of 2Al₂O₃ and Ti₃Al. The relative density of the composite was 99.5%. The average hardness and fracture toughness were 1340 kg/mm² and 8 MPa·m^1/2, respectively.     

Effect of Milling Time on Electrical Breakdown Behavior of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/Cu Composite

In order to clarify the relationship between the microstructure and the arc erosion behavior of metal-matrix composite, Al₂O₃/Cu composites with different distributions of Al₂O₃ particles were prepared by high energy ball milling and powder metallurgy. The effect of milling time on microstructure, properties, and arc erosion behavior of Al₂O₃/Cu composite was investigated. The results show that the distribution of Al₂O₃ particles improves significantly with increase of milling time, but Al₂O₃ particles will be aggregated if milling time is too long. The optimal milling time is 24 h in the range of experiments. A uniform distribution of Al₂O₃ particles in copper matrix can improve the hardness, electrical conductivity, average breakdown strength, chopping level, and arc life. With improvement in the distribution of Al₂O₃ particles, the erosion area becomes larger, and the erosion pits become shallower and are dispersed more uniformly.     

Effect of partial substitution of calcium for yttrium on the structure and properties of the Y<Subscript>0.9</Subscript>Ca<Subscript>0.1</Subscript>Ba<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>6.8</Subscript> superconductor

The crystal structure of the high-temperature Y_1–xCa_xBa₂Cu₃O_6.8 superconductor has been studied in a temperature range of 80–300 K using low-temperature X-ray diffraction analysis; its microstructure has been studied by scanning and transmission electron microscopy. Changes of the bond length in the structure of principal phase and precipitation topology of impurity phases and their compositions have been analyzed. An addition of calcium was shown to increase the environmental tolerance of the principal Y123 phase and its microhardness and ensures the low unchanged coefficient of thermal expansion. All of the facts indicate that the material can be used to manufacture composite superconducting articles.     

Characterization of Thermal-Sprayed HAP and HAP/TiO<Subscript>2</Subscript> Coatings for Biomedical Applications

In the present study, hydroxyapatite (HAP) coating along with HAP/TiO₂ coating has been deposited by high-velocity flame spray (HVFS) technique onto 316LSS. Titania was used as a bond coat and HAP as top coat in HAP/TiO₂ coating. The main aim of the study is to investigate the corrosion behavior of thermal spray coating of HAP and HAP/TiO₂ on steel. Electrochemical corrosion testing was carried out using potentiodynamic polarization test. The corrosion behavior of bare and as-sprayed specimens was analyzed in simulated body fluid known as Hank’s solution. As-sprayed specimens along with corroded specimens were further characterized by XRD, SEM/EDS, and x-ray mapping analysis. It was observed that the HAP/TiO₂ coating possessed higher microhardness (280 Hv) as compared to HAP coating (254 Hv). Surface roughness also got enhanced in case of HAP/TiO₂ coating (9.35 μm) as compared to pure HAP coating (7.37 μm). The porosity of the HAP coating was found to be higher than the bond coating. It was observed that the Ca/P ratio almost resembled that of the natural bone composition. The corrosion resistance of steel increased after the deposition of HAP and HAP/TiO₂ coatings. The maximum corrosion resistance was exhibited by HAP/TiO₂ coating.