Fabrication of dense thin sheets of γ-TiAl by hot isostatic pressing of tape-cast monotapes

A method is described for the fabrication of dense thin sheets of γ titanium aluminide (γ-TiAl) by a powder metallurgy route involving hot isostatic pressing (HIP) of tape-cast monotapes. Gamma-TiAl powder (particle size <90 μm) was incorporated into a concentrated slurry by mixing with an organic binder in a solvent and the system was tape-cast to form sheets with a thickness of 400–600 μm. After insertion of the tape-cast sheet into a HIP can and binder removal in situ by thermal decomposition, HIP at 1100 °C under a pressure of 130 MPa produced dense sheets with a thickness of 250–400 μm. The free, dense sheets with a fine-grain microstructure were obtained by dissolution and oxidation of the HIP can. The carbon content of the fabricated sheets was 0.035 wt.%. Facile adaptation of the process to the production of γ-TiAl thin sheets with complex shapes is expected.     

Formation of Al2Cu and AlCu intermetallics in Al(Cu) alloy matrix composites by reaction sintering

We report the fabrication and characterization of a series of Al(Cu) alloy-based matrix composites. The composites were produced by sintering and rapid quenching three powder mixtures of Al and Cu with hypoeutectic, eutectic, and hypereutectic compositions. The morphology of the reinforcements formed in the Al(Cu) matrices of these composites was found to be variable. A two-phase Al₂Cu–Al(Cu) nanoeutectic, with lamellar spacing of 200–300 nm, was found in the Al(Cu) matrix of the sample having hypoeutectic composition after it was oil-quenched from 1000 °C to room temperature. While oil quenching the sample with eutectic composition, produced single Al₂Cu crystals of 2–2.5 μm size, embedded in a lamellar nanoeutectic matrix. As for the hypereutectic alloy, the matrix of the oil-quenched sample consisted mainly of Al₂Cu intermetallic, and a secondary phase of AlCu dendrites with dendrite arms spacing of 1–1.5 μm.     

Hot Isostatic Pressing of MgAl2O4 Spinel Infrared Windows

Optically transparent MgAl₂O₂ spinels have been produced by hot isostatic pressing (HIP). The spinel samples were prepared by hot pressing and subjected to capsule-free HIPing. The hot-pressed samples were made at 1500°C with a pressure from 14 to 41 MPa for 2 to 4 hours. In the HIP process, the pressure ranged from 14 to 207 MPa at 1500°C. The effect of hot isostatic pressure on the bulk density, microstructure and optical properties of the spinel sample were investigated here. The bulk density of the sample increased with HIP pressure and the sample HIPed at 207 MPa resulted in a bulk density of 3·576 g/cm³, about 99·94% of the theoretical density. A bimodal grain size distribution exists in samples HIPed at pressures ≤ 138 MPa. The extent of the abnormal grain growth decreased with pressure. The transparent spinel with uniform and fine grain size of 2 μn was obtained at 207 MPa. The transmission at short wavelength increased significantly with HIPing pressure. The transmittance of the sample HIPed at 207 MPa at a wavelength of 0·7 μn was 72%.     

Change in grain size and flow strength in P/M Rene 95 under isothermal forging conditions

The changes in microstructure induced by plastic deformation in hot isostatically pressed (HIPed) P/M Rene 95 under isothermal conditions are discussed. Results of the constant true strain rate compression tests are presented for initially fine (7 μm) and coarse (50 μm) grained compacts deformed at temperatures of 1050 °C, 1075 °C and 1100 °C and at strain rates in the range from 10⁻⁴ s⁻¹ to 1 s⁻¹. Under these test conditions, both the fine and coarse-grained compacts recrystallize and their grain size are refined during flow. This grain refinement gives rise to softening in both materials. Ultimately, their microstructures transform into the same equiaxed fine-grained microduplex structure at which point their flow strength becomes identical. Continued deformation at that point produces no further change in grain size or flow strength. Under this steady state regime of deformation, the microduplex grain size and flow strength are independent of the original microstructure but are conditioned by the strain rate at a given temperature. The steady state grain size increases whereas the steady flow strength decreases with a decrease in strain rate and/or an increase in temperature.     

Effect of γ′ precipitation during hot isostatic pressing on the mechanical property of a nickel-based superalloy

The effect of the precipitation of γ′ phase during hot isostatic pressing (HIPing) on the mechanical property of a nickel-based superalloy, GTD-111, was evaluated by conducting tensile and creep-rupture tests at 871 °C. In the 4-h two-step HIP process, the coupons were isostatically compressed (at 120 MPa) and heated to 1230 °C, well above the dissolution temperature of γ′ precipitates into the γ matrix, for the first 2 h, and cooled down to a temperature to induce the precipitation of γ′ phase and held for the last 2 h at 120 MPa or at ambient pressure. The precipitates were controlled in size by varying the temperature for the last half of the process. According to the result of the tensile test, the mechanical properties of the alloy were varied upon the microstructural evolution, and improved more than 40%, compared to those of the untreated ones. The precipitation of γ′ phase under high pressure further improved in the properties, suggesting that the precipitation of γ′ phase at high pressure provides an advantage for the rigidity of the structure. Based on these findings, a 6-h three-step HIP process was tried, and proved to be an effective substitute for the normal heat treatment, especially in terms of creep properties. This feature was mostly attributed to the homogenized microstructure of HIPed ones, as evidenced by the X-ray diffraction patterns.     

Effect of hydrogen radical on growth of μc-Si in hetero-structured SiCx alloy films

The changes of the crystallinity of μc-Si phase are studied in samples deposited with hydrogen dilution ratio, H₂/SiH₄, from 9.0 to 19.0 by hot-wire CVD (Cat-CVD). In the samples deposited at filament temperature, T_f, of 1850 °C, the crystalline fraction and the crystallite size of μc-Si phase increased with increasing the H₂/SiH₄. The carbon content, C/(Si+C), was almost constant. In the XRD patterns, the intensity of Si(1 1 1) peak decreased and that of Si(2 2 0) peak increased with increasing the H₂/SiH₄. In the samples deposited at T_f of 2100 °C with H₂/SiH₄ over 11.4, the μc-Si phase was not formed and the C/(Si+C) increased. The growth mechanism of μc-Si in hetero-structured SiC_x alloy films is discussed.     

Microstructural characterization of P/M Ni3Al consolidated by HIP

Rapidly solidified powder of Ni₃Al doped with boron was produced by inert gas atomization and consolidated by hot isostatic pressing (HIP). Morphology and microstructure of the powder were studied. From the particle morphology, it could be deduced that the solidification time was similar at least to the time necessary for complete fragmentation of the liquid. The powder showed a two-phase microstructure that was finer the smaller the particle size. The presence of dendrites of NiAl (β) phase was consistent with the diagram proposed by Schramm and not with the traditional diagram of Singleton et al. The microstructure of the material consolidated at 1100°C and 1200°C was studied. A monophasic structure was observed after HIP, and no relevant microstructural differences were seen between the two temperatures used.     

EBSD analysis of a Ti-IF steel subjected to hot torsion in the ferritic region

The effect of grain size on the warm deformation behaviour of a titanium stabilized interstitial free steel was investigated using hot torsion. Tests were performed at temperatures between 765 °C and 850 °C at strain rates between 0.003 s⁻¹ and 1 s⁻¹ for samples with grain sizes of 25 μm, 75 μm and 150 μm. The structures were observed using EBSD analysis and are consistent with those expected for materials dominated by dynamic recovery. Some evidence was found for small amounts of thermally induced migration of pre-existing boundary (bulging) and for the generation of new segments of high angle boundaries by continuous dynamic recrystallization. The early onset of a steady-state flow stress in the finer grained samples is attributed to one or a combination of thermally induced boundary migration and enhanced rates of recovery near subgrain (and grain) boundaries.     

Vacuum heat treatment of LiAlO2 densified silicon nitride ceramics

The aim of the present work has been to produce high-dense Si₃N₄ ceramics by a cheaper pressureless sintering method and then to attain vacuum heat treatment to remove residual grain boundary glass in gaseous form. LiAlO₂ was used as a sintering additive rather than using Li₂O, since its grain boundary glass is not stable above 1200 °C. LiAlO₂ was synthesised from 42% Li₂CO₃ and 58% Al₂O₃ powder mix reacting together at 1450 °C for 3 h in a muffle furnace. X-ray analysis showed that 95% LiAlO₂ was obtained. LiAlO₂ was milled and added to silicon nitride powder as a sintering additive. Hot-pressing and pressureless sintering of LiAlO₂ containing Si₃N₄ compacts were carried out at temperatures between 1450–1750 °C. The sintered samples were vacuum heat-treated at elevated temperatures under high vacuum to remove intergranular glass and to increase refractoriness of Si₃N₄ ceramics. Scanning electron microscope images and weight loss results showed that Li in grain boundary glass (Li–Al–Si–O–N) was successfully volatilised, and oxidation resistance of the sintered samples was increased.     

Strength and toughness of beryllium-niobium intermetallic compounds

Bend and compression strengths, fracture toughness, and high-temperature microhardness of Be---Nb intermetallic compounds were measured at temperatures up to 1200 °C. Be₁₂Nb and Be₁₇Nb₂ materials exhibited brittle behavior at temperatures below 1100 °C in bending and below 800 °C in compression. Hot isostatically pressed (HIP) Be₁₂Nb had the highest low-temperature strengths (250 MPa in bending and 2750 MPa in compression) resulting from its greater fracture toughness (K_IC = 4 MPa m^1/2) compared with the other Be---Nb materials, vacuum hot pressed (BHP) Be₁₂Nb, and HIP Be₁₇Nb₂, which had . Measured strengths for the HIP Be₁₂Nb were more than twice that measured for the VHP Be₁₂Nb or for HIP Be₁₇Nb₂. The HIP Be₁₂Nb also exhibited good high-temperature mechanical properties, having a bend strength of 250 MPa at 1200 °C, compared with less than 100 MPa for the VHP Be₁₂Nb. However, intergranular embrittlement was observed at intermediate temperatures, reducing the HIP Be₁₂Nb bend strength and fracture toughness below those measured for the other materials. HIP Be₁₇Nb₂ exhibited poor low-temperature properties, but high-temperature bend strengths of 740 MPa at 1100 °C and 400 MPa at 1200 °C were measured. Strength in compression was similar for all materials above 800 °C, decreasing sharply to about 600 MPa at 1000 °C and to 200 MPa at 1200 °C. Microhardness and indentation creep tests also revealed similar high-temperature behavior among the materials. Power-law creep exponents ranging from 4.1 to 6.6 and activation energies of 220–290 kJ mol⁻¹ were measured for the beryllides, with the HIP Be₁₂Nb having the highest activation energy for creep.     

Templated grain growth of SrBi2Ta2O9 ceramics: Mechanism of texture development

Textured SrBi₂Ta₂O₉ (SBT) ceramics were fabricated via templated grain growth (TGG) technique using platelet-like SBT single crystal templates. The templates (5 wt%) were embedded in a fine-grain SBT powder matrix containing 3 wt% of Bi₂O₃ excess that were subjected to uniaxial pressing and sintering at 1000–1250 °C for up to 24 h. Microstructural characterization by SEM was performed to establish the effect of sintering parameters on the grain growth and texture development. It was found that the ceramics developed a bimodal microstructure with notable concentration of large (longer than 90 μm) aligned grains with c-axis oriented parallel to the pressing direction. The mechanism controlling the texture development and grain growth in SBT ceramics is discussed.     

Infrared Transmission Curves of Pb0.1 Ca0.9La2S4 Pellets Densified by Pressureless Sintering

Highly sinterable submicron Pb_0.l Ca_0.9La₂S₄(PCLS) powders were prepared by sulfidizing calcium and lanthanum alkoxides al 500°C under CS, atmosphere for 8 hours and then in pure H₂S atmosphere at 600-800°C for 8 hours. After sintering the pellets were used as infrared transmitting window material of 8-14 μm wavelength. The CdS was added from 3 to 7 wt.% lo improve the sinterability by forming liquid phase during sintering. For sulfidization of lanthanum alkoxide, sulfide powder with LaS₂ phase was formed at 500°C, and a pure Th3P4 phase formed follow by 700°C heat treatment. A powder with β-La₂S₃phase formed at 800°C, and a pure Th₃ P₄phase formed follow by 900°C heat treatment. The powder with β-La₂S₃ phase was sintered to full density at 1350°C by adding 3 wt.% CdS. The PCLS powder with Th3P4 phase sintered to full density at 1400°C by also adding 3 wt.% CdS. The pellet exhibited 45% transmittanceat 13 μm when sintered from the powder with p-La₂S₃phase. The transmittance at 2.5 μm for the pellet sintered from the PCLS powder with Th₃P₄ type structure was 3 times higher than that from the p-La₂S₃ powder.     

Tungsten chemical vapor deposition using tungsten hexacarbonyl: microstructure of as-deposited and annealed films

Tungsten (W) films were deposited on Si(100) from tungsten hexacarbonyl, [W(CO)₆], by low-pressure chemical vapor deposition (CVD) in an ultra-high vacuum (UHV)-compatible reactor. The chemical purity, resistivity, crystallographic phase, and morphology of the deposited films depend markedly on the substrate temperature. Films deposited at 375°C contain approximately 80 at.% tungsten, 15 at.% carbon and 5 at.% oxygen. These films are polycrystalline β-W with a strong (211) orientation and resistivities of >1000 μΩ cm. Vacuum annealing at 900°C converts the metastable β-W to polycrystalline -W, with a resistivity of approximately 19 μΩ cm. The resultant -W films are porous, with small randomly oriented grains and nanoscale (<100 nm) voids. Films deposited at 540°C are high-purity (>95 at.%) polycrystalline -W, with low resistivities (18–23 μΩ cm) and a tendency towards a (100) orientation. Vacuum annealing at 900°C reduces the resistivity to approximately 10 μΩ cm, and results in a columnar morphology with a very strong (100) orientation.     

Domain patterns on ferroelectric Rh:BaTiO3 single crystals

Single crystal growth and domain structure of Rh:Barium titanate (BaTiO₃) have been investigated. Rh doping in BaTiO₃ is effective for the growth of bulk crystals without twin formation. Atomic force microscope (AFM) and optical microscope studies reveal the formation 180° and 90° domains on the grown crystals. It has been observed that the complex 180° domain structure with typical size of around 20 μm exists in the c-domain of {0 0 1} face of Rh doped BaTiO₃ crystals.     

Sintering kinetics of 8Y–cubic zirconia: Cation diffusion coefficient

Zirconia ceramics, mainly of cubic phase, are used in different applications because of their particular electrical and structural properties.

After the forming stage, sintering leads to a material with suitable microstructural characteristics. The sintering process mainly depends on thermal cycle and on starting particle size and its distribution; it also depends on density and the microstructure of green material. Cubic zirconia has a high (2680 °C) melting temperature; however, effective sintering could be observed for temperatures higher than 900 °C (nanoparticles), and it may reach a final density of 96–98% the theoretical value at relative low temperatures.

The objective of this paper is to study the sintering kinetics of stabilized zirconia in its cubic phase with 8% molar of Y₂O₃ under fast firing rates up to nearly isothermal conditions. Samples were shaped from suspensions dispersed with ammonium polyacrylate by slip casting. Sintering was performed in the temperature range between 1200 °C and 1400 °C. The sintering kinetic process was followed by measuring density as a function of time. A sintering model was applied to fit the experimental data of the first steps of densification. It was observed that sintering obeys the same mechanism in the temperature and time ranges under study, which results in an activation energy of 170 kJ mol⁻¹. Sintering is controlled by Zr cation diffusion, for which a lattice diffusion coefficient of D_l = 8 × 10⁻¹² cm² s⁻¹ at 1400 °C was found, and the activation energy of the diffusion process was 223 kJ mol⁻¹.     

Time resolved luminescence of quartz from Nigeria

Characteristics of luminescence lifetimes and luminescence intensity obtained from time resolved spectra of quartz from Nigeria are presented. The luminescence was pulse-stimulated at 11 μs width at 470 nm. Samples used consisted of unannealed quartz as well as samples annealed at 500 °C, 600 °C, 700 °C, 800 °C and 900 °C. The luminescence lifetimes and luminescence intensities were studied as a function of annealing temperature, irradiation dose and measurement temperature. It was found that there is a decrease, although non-monotonic, in the luminescence lifetime with change in annealing temperature from 20 to 900 °C. In addition, lifetimes extracted from time resolved spectra of unannealed samples as well as ones annealed at 500 °C and 600 °C are initially independent of irradiation dose but do later decrease with further irradiation. Regarding the luminescence intensity it was observed that in general, the intensity passes through a peak as the measurement temperature is increased from 20 to 200 °C with slight differences in the detailed pattern dependent on preheating. Activation energies for thermal quenching and thermal assistance evaluated from temperature-dependent changes of luminescence lifetime and luminescence intensity are given. The results are discussed in terms of a model consisting of three luminescence centres with probability of hole trapping during irradiation being highest for the luminescence centre associated with the least lifetime.     

Physical models for cleavage fracture at various temperatures—Bases for local approach to fracture of HSLA steel

The author proposes the critical events controlling cleavage at various temperatures: at a very low temperature (−196 °C), critical event is the nucleation of a crack in ferrite at the precrack tip. At a moderate low temperature (around −100 °C), the critical event is the propagation of a carbide crack into the ferrite grain. With increasing temperature (around DBTT −80 °C), the carbide crack eligible to propagate into the ferrite grain should be the one initiated by a critical strain higher than that to initiate a carbide crack at low temperatures. The higher critical strain increases the flow stress by work hardening for making up the effect of lowering yield stress. At a higher temperature (−30 °C) after the crack tip is blunted to more than 60 μm and a fibrous crack extends, the critical event for cleavage fracture is the propagation of a grain-sized crack.     

Production of a highly porous material by liquid phase sintering of short ferritic stainless steel fibres and a preliminary study of its mechanical behaviour

A procedure is outlined for the production of highly porous material by liquid phase sintering of short stainless steel fibres, about 100 μm in diameter. The fibres, which were produced by a melt extraction route, were first electroplated with copper to a thickness of a few μm. The sintering procedure was then completed by holding at about 1100 °C for a few minutes. It is shown that this operation generates strong joints by the migration of liquid copper to the fibre–fibre contact regions, as a result of capillary action. A preliminary study of the mechanical behaviour material produced in this way indicates that its toughness is relatively high, for a highly porous metallic material, and that its fracture energy is broadly consistent with predictions from a model based on evaluation of the work done by plastic deformation and rupture of individual fibres close to the fracture plane.     

Piezoelectric and dielectric properties of PZT–PZN–PMS ceramics prepared by molten salt synthesis method

Piezoelectric powders and ceramics with the composition of Pb_0.95Sr_0.05(Zr_0.52Ti_0.48)O₃–Pb(Zn_1/3Nb_2/3)O₃–Pb(Mn_1/3Sb_2/3)O₃ (PZT–PZN–PMS) were prepared by molten salt synthesis (MSS) and conventional mixed-oxide (CMO) methods, respectively. The influence of synthesis process on the properties of powders and ceramics were investigated in detail. The results show that the MSS method significantly improved the sinterability of PZT–PZN–PMS ceramics, resulting in an improvement of dielectric and piezoelectric properties compared to the CMO method. The optimum values of MSS samples are as follows: _r = 1773; tan δ = 0.0040; T_c = 280 °C; d₃₃ = 455 pC/N; k_p = 0.70; Q_m = 888; E_c = 10.3 kV/cm; and P_r = 28.2 μC/cm², at calcination of 800 °C and sintering of 1120 °C temperature.     

Diffusion bonding between commercially pure titanium and micro-duplex stainless steel

Diffusion-bonded joints between commercially pure titanium and micro-duplex stainless steel were prepared in the temperature range of 800–950 °C for 1.5 h under 3 MPa uniaxial load in vacuum. The diffusion bonds were characterized using light and scanning electron microscopy. The composition of the reaction products were determined by energy dispersive spectroscopy. Up to 850 °C, -Fe + λ and λ + FeTi phase mixtures were formed at diffusion interface; however -Fe + λ, λ + FeTi and FeTi + β-Ti phases mixtures were formed at 900 °C and above. The presence of these intermetallics was confirmed by X-ray diffraction technique. The maximum tensile strength of 96% of Ti and shear strength of 81% of Ti along with 6.9% ductility were obtained for the diffusion couple processed at 850 °C due to the finer width of intermetallic phases. With a rise in the joining temperature the bond strength drops owing to an increase in the width of reaction products.