Studies on the development of TZM alloy by aluminothermic coreduction process and formation of protective coating over the alloy by plasma spray technique

TZM alloy is a potential candidate for high temperature structural applications. However, in the preparation of this alloy by conventional melt-casting route, difficulties are encountered in achieving homogenized alloy composition in view of high melting temperature of the alloy and presence of minor alloying components. Therefore, an alternative technique of aluminothermic co-reduction was adopted to prepare TZM alloy of composition, Mo-0.5Ti-0.1Zr-0.02 °C, wt.% by simultaneous reduction of uniformly premixed oxides of MoO₂, TiO₂ and ZrO2 by aluminium in presence of requisite amount of carbon. The as-reduced alloy was further arc melted for consolidation. Since, TZM alloy is by nature highly susceptible to oxidation at elevated temperature in air or oxygen, therefore feasibility of development of silicide type of coating over the synthesized alloy by plasma coating technique was also examined. Silicon powder coated on TZM alloy surface by plasma spray technique was finally converted into MoSi₂ coating by sintering at 1350 ^°C for 2-4 h duration under argon. A double layer coating structure was formed with two distinct phases. The inner thin layer was consisted of Mo₂Si₅ phase (~ 10 μm) followed by thick outer layer of MoSi₂ (~ 150 μm). The coating showed good adhesion strength and stable oxidation with negligible mass gain (10 g/m²) at 1000 ^°C in air.     

W–15 wt%Cu nano-composite produced by hydrogen-reduction/sintering of WO3–CuO nano-powder

A two-stage hydrogen-reduction/sintering procedure was used to synthesize W–15 wt%Cu nano-composite tablets. Hydrogen-reduction was carried out at 600, 650, 700 and 750 °C for 15–90 min and sintering was performed at 1100, 1150, 1200 and 1250 °C for 60 min. Morphology and grain size of the products were rigorously investigated by scanning electron microscope (SEM), X-ray diffractometer (XRD) and nano-particle Zeta-sizer. Maximum consolidation of the nano-composite product was achieved at 1200 °C. Hydrogen-reduction at 700 °C for 90 min showed an average particle size of ∼72.9 nm. Total reduction was achieved at higher temperatures and longer times. The mixture had a homogeneous structure with 16.1 ± 0.1 g/cm³ density when sintered at 1200 °C for 60 min.     

Fabrication of full density near-nanostructured cemented carbides by combination of VC/Cr3C2 addition and consolidation by SPS and HIP technologies

The aim of present work is to study the effect of VC and/or Cr₃C₂ in densification, microstructural development and mechanical behavior of nanocrystalline WC-12wt.%Co powders when they are sintered by spark plasma sintering (SPS) and hot isostatic pressing (HIP). The results were compared to those corresponding to conventional sintering in vacuum. The density, microstructure, X-ray diffraction, hardness and fracture toughness of the sintered materials were evaluated. Materials prepared by SPS exhibits full densification at lower temperature (1100 °C) and a shorter stay time (5 min), allowing the grain growth control. However, the effect of the inhibitors during SPS process is considerably lower than in conventional sintering. Materials prepared by HIP at 1100 °C and 30 min present full densification and a better control of microstructure in the presence of VC. The added amount of VC allows obtaining homogeneous microstructures with an average grain size of 120 nm. The hardness and fracture toughness values obtained were about 2100 HV₃₀ and close to 10 MPa m^1/2, respectively.     

Synthesis of ultrafine/nanocrystalline W-(30-50)Cu composite powders and microstructure characteristics of the sintered alloys

Ultrafine/Nanocrystalline W-Cu composite powders with various copper contents (30, 40 and 50 wt.%) have been synthesized by sol-spray drying and a subsequent hydrogen reduction process. The powders were consolidated by direct sintering at temperatures between 1150 and 1260 °C for 90 min. The powder characteristics and sintering behavior, as well as thermal conductivity of the sintered alloys were investigated. The results show that the synthesized powders exist in ultrafine composite particles containing numerous nanosized particles, and the composition distributed very homogeneously. As the copper contents increase, the grain size of the powders decreases. The subsequent sintered parts show nearly full density with the relative density more than 99% at the temperature of 1250 °C. The sintered parts have very fine tungsten grains embedded in a bulk matrix. With increased copper contents, the tungsten grain size decreases and the microstructural homogeneity of the sintered alloys improves further. The thermal conductivity properties, while a little lower than that of the theoretical value, depend on the copper contents.     

Effect of SPS process sintering on the microstructure and mechanical properties of nanocrystalline TiC for tools application

The most important spark plasma sintering (SPS) parameters (Temperature, holding time and pressure), have been reviewed to assess their effect on the densification, grain growth kinetics and mechanical properties of nanocrystalline TiC synthesized by mechanical alloying. Experiments were performed in the 1350-1800 °C temperature range with holding time from 1 to 10 min under various pressure values of 50, 80 and 100 MPa. The results of experiments revealed that the mechanical properties of the material were improved with raising the sintering temperature and extending the sintering time. However, a hardness decrease was observed as a result of abnormal grain growth under higher sintering temperatures. The optimized process parameters for SPS process are identified as a sintering temperature of 1650 °C, a pressure 100 MPa and a sintering time of 5 min. The resulting mechanical properties are: a relative density of 97.9%, a micro-hardness of 2570 Hv, a nano-hardness of 28 GPa, a fracture toughness of 4.9 MPa·m^1/2 and a compressive strength of about 2210 MPa.     

Oxidation protection of gamma-titanium aluminide using glass-ceramic coatings

γ-TiAl intermetallic alloys are presently considered an efficient structural material for advanced turbine blades and aero-engine components due to their various advantages compared to the traditionally used superalloys. However, their poor oxidation resistance at temperatures > 750 °C severely limits their wider application. The present study dealt with the improvement of oxidation resistance of this alloy by applying impervious glass-ceramic coatings by vitreous enameling technique. Results showed that MgO-SiO₂-TiO₂ glass-ceramic coating could offer excellent oxidation resistance to γ-TiAl at 800 °C even up to 100 h with negligible weight gain (~ 0.10 mg/cm²) compared to that of the bare alloy (~ 1.3 mg/cm²). The coatings those were belonging from BaO-MgO-SiO₂, ZnO-Al₂O₃-SiO₂ and BaO-SiO₂ systems also extend appreciable improvement in the oxidation resistance of the alloy at 800 °C up to 100 h. At further higher temperature such as at 1000 °C, the ABK-13 and ABK-103 glass-ceramic coatings offered significant protection to the alloy up to 25 h of exposure in air with minimum weight gain (~ 0.34 mg/cm²). However, after that the coated layers started to peel off from the alloy surface.     

The effect of consolidation parameters on the mechanical properties of binderless tungsten carbide

This paper discusses the effect of the process parameters on the mechanical properties of binderless pure tungsten carbide during a GPS (gas protection sintering) process. The result of experiments reveal that the mechanical properties of the material increases with raising the sintering temperature and extending the retention time; however a decreased hardness was observed as a result of abnormal grain growth under higher sintering temperatures. The results of XRD and EDS analyses confirmed the absence of brittle phases such as W₂C or impurity phases in the microstructure. The optimized process parameters for GPS process are identified as: a mean particle size of 1.03 μm, a sintering temperature of 1860 °C and a retention time of 60 min; the resulting mechanical properties are: a relative density of 95.1%, a micro-hardness of 1718 kgf/mm² and a fracture toughness of 5.97 MPa m^1/2. The width of particles size distribution has a significant effect on the density and hardness of the sintered material however the width of particles size distribution is dependent on the original particle size. Finally, ultra-fine particles increase the chance of conglomeration and sub-micron structures. The conglomeration of ultra-fine particles hinders the filling of porosities during sintering and lowers the density and hardness of the material.     

Producing nanocrystalline bulk Mg-3Al-Zn alloy by powder metallurgy assisted hydriding-dehydriding

Nanocrystalline bulk Mg-3Al-Zn alloy with an average grain size of 48 nm has been prepared by powder metallurgy assisted hydriding-dehydriding. Evolutions of nanograined structure powders and bulk alloy have been investigated by TEM, SEM and XRD, respectively. The results showed that by milling in hydrogen for 60 h, as-hydriding powder possessed an average grain size of 5.9 nm. After a subsequent process of desorption-recombination treatment (at 350 °C) and consolidation process (extruded at 200 °C) resulted in bulk samples with an average crystallite size of 48 nm and MgH₂ was fully turned into Mg. The consolidated samples of 60 h milled powder had a final density of 1.77663 ± 0.006 g/cm³, which corresponded to 97.57 ± 0.3% of theoretical density. The highest microhardness of the nanocrystalline bulk alloy reached about 872.5 MPa, which is about three times higher than that of the coarse-grained AZ31.     

Investigation of interfacial properties of atmospheric plasma sprayed thermal barrier coatings with four-point bending and computed tomography technique

A modified four-point bending test has been employed to investigate the interfacial toughness of atmospheric plasma sprayed (APS) yttria stabilised zirconia (YSZ) thermal barrier coatings (TBCs) after isothermal heat treatments at 1150 °C. The delamination of the TBCs occurred mainly within the TBC, several to tens of microns above the interface between the TBC and bond coat. X-ray diffraction analysis revealed that the TBC was mainly tetragonal in structure with a small amount of the monoclinic phase. The calculated energy release rate increased from ~ 50 J/m^− 2 for as-sprayed TBCs to ~ 120 J/m^− 2 for the TBCs exposed at 1150 °C for 200 h with a loading phase angle about 42°. This may be attributed to the sintering of the TBC. X-ray micro-tomography was used to track in 3D the evolution of the TBC microstructure non-destructively at a single location as a function of thermal exposure time. This revealed how various types of imperfections develop near the interface after exposure. The 3D interface was reconstructed and showed no significant change in the interfacial roughness after thermal exposure.     

Microstructure Modification of Powder Compact of Al-Zn-Mg Nanostructured Alloy by a Semisolid Thermomechanical Processing

A thermomechanical process(TMP) consisting of three cycles of cold pressing at 154 MPa and liquid-phase sintering at 600 ℃ for 30 min in each cycle was applied to modify the microstructure of nanostructured Al-Zn-Mg alloy.The alloy powders were produced by mechanical alloying.Also,solid-state sintering at 550 ℃ for 90 min was done to compare the results with those obtained from the TMP.The powders and the thermomechanically(TM) processed samples were analyzed by XRD to reveal the present phases in addition to calculating the crystallite size changes by the Williamson-Hall method.Moreover,scanning electron microscope was employed to observe the morphology of the powder and the microstructures of the sintered and the TM processed samples.The results revealed that the TMP affected the microstructure noticeably as well as the microhardness by removing the continuous grain boundary porosities and uniform distribution of the intermetallic phase particles as well as obtaining a near globular microstructure after the second cycle.Also,the average grain sizes in the first and the second cycles of the TMP were lower than those of the sintered sample.Furthermore,nanocrystalline grains were stable up to the second cycle of the TMP.