MA Al alloys are examined to determine the effects of alloying of Mg and Cu and rolling on tensile deformation behavior at 748 K over a wide strain rate range(10−4-103/s). A powder metallurgy aluminum alloy produced from mechanically alloyed pure Al powder exhibits only a small elongation-to-failure(εf < ~50%) in high temperature(748 K) tensile deformation at high strain rates( = 1-102/s). εf in MA Al-0.5~4.0Mg alloys increases slightly with Mg content(εf = ~140% at 4 mass%). Combined addition of Mg and Cu(MA Al-1.5%Mg-4.0%Cu) is very effective for the occurrence of superplasticity(εf > 500%). Warm-rolling(at 393-492 K) tends to raise εf. Lowering the rolling-temperature is effective for increasing the ductility. The effect is rather weak in MA pure Al and MA Al-Mg alloys, but much larger in the MA Al-1.5%Mg-4.0%Cu alloy. Additions of Mg and Cu and warm-rolling of the alloy cause a remarkable reduction in the logarithm of the peak flow stress at low strain rates ( < ~1/s) and sharpening of microstructure and smoothening of grain boundaries. Additions of Mg and Cu make the strain rate sensitivity(the m value) larger at high strain rates, and the warm-rolling may make the grain boundary sliding easier with less cavitation. Grain boundary facets are observed on the fracture surface when εf is large, indicating the operation of grain boundary sliding to a large extent during superplastic deformation.

Binary Ti-Al alloys below 51.0 mass%Al content exhibit a breakaway, transferring from parabolic to linear rate law. The second Al2O3 layer might have some protectiveness before breakaway. Ti-63.1 mass%Al oxidized at 1173 K under parabolic law. Breakaway oxidation is observed in every alloy, except for Ti-63.1 mass%Al. After breakaway, oxidation rates of the binary TiAl alloys below 34.5 mass%Al obey almost linear kinetics. The corrosion rate of Ti-63.1 mass%Al appears to be almost parabolic. As content greater than 63.0 mass% is found to be necessary to form a protective alumina film. Addition of Mo improves the oxidation resistance dramatically. No breakaway is observed at 1123 K, and breakaway is delayed by Mo addition at 1173 K. At 1123 K, no breakaway, but a parabolic increase in mass gain, are observed in the Mo-added TiAl alloys. The binary Ti-34.5 mass%Al exhibits a transfer from parabolic to linear kinetics. At 1173 K, the binary alloys show vary fast linear oxidation and even the Mo-added alloys exhibit breakaway oxidation. The 2.0 mass%Mo-added TiAl exhibits a slope between linear and parabolic. At values of 4.0 and 6.0 mass% added TiAl alloys, slightly larger rates are observed than those for the parabolic rate law, even after breakaway. On those alloys, the second Al2O3 layer appears to be persistently continuous. Oxidation resistance is considerably degraded by the addition of Mn. Mn appears to have the effect of breaking the continuity of the second Al2O3 layer.

Crystal structure of the L12 type (Al,X)3Ti alloy (X = Cr,Cu) is analyzed by X-ray diffractometry and the nonuniform strain behavior at high temperature is investigated. The lattice constants for the L12 type (Al,X)3Ti alloys decrease in the order of the atomic number of the substituted atom X, and the hardness tends to increase. In a compressive test at around 473K for Al67.5Ti25Cr7.5, Al65Ti25Cr10 and Al62.5Ti25Cu12.5 alloys, it is found that the stress-strain curves showed serration, and deformation rate dependence appeared. It is assumed that the generation of serration is due to dynamic strain aging caused by the diffusion of solute atoms. As a result, activation energy of 60-95 kJ/mol is obtained. This process does not require direct involvement. In order to investigate the generation of serrations in detail, compression tests are carried out under various conditions. As a result, in the strain rate range of this experiment, serration is found to occur after 470K at a certain critical strain. The critical strain increases as the strain rate increases at constant temperature, and the critical strain tends to decrease as temperature rises under constant strain rate. This tendency is common to all alloys produced. In the case of this alloy system, the serration at around 473K corresponds to the case in which the dislocation velocity is faster than the diffusion rate of interstitial solute atoms at low temperature.

In order to increase the efficiency of the sputtering method widely used in thin film fabrication, a dc sputtering apparatus which supplies both high frequency and magnetic field from the outside was fabricated, and cobalt thin film was fabricated using this apparatus. The apparatus can independently control the applied voltage, the target-substrate distance, and the target current, which are important parameters in the sputtering method, so that a stable glow discharge is obtained even at a low gas pressure of 10−3 Torr. The fabrication conditions using the sputtering method were mainly performed in Ar+O2 mixed gas containing about 0.6% oxygen gas under various Ar gas pressures of 1 to 30 mTorr. The microstructure of Co thin films deposited using this apparatus was examined by electron diffraction pattern and X-ray techniques. The magnetic properties were investigated by measuring the magnetization curves. The microstructure and magnetic properties of Co thin films depend on the discharge gas pressure. The thin film fabricated at high gas pressure showed a columnar structure containing a large amount of the third phase in the boundary region and the thin film formed at low gas pressure showed little or no columnar structure. The coercivity in the plane was slightly larger than that in the latter case.

N-type porous silicon (PS) layers and thermally oxidized PS layers have been characterized by various measuring techniques such as photoluminescence (PL), Raman spectroscopy, IR, HRSEM and transmittance measurements. The top surface of PS layer shows a stronger photoluminescence peak than its bottom part, and this is ascribed to the difference in number of fine silicon particles of 2~3 nm in diameter. Observed characteristics of PL spectra are explained in terms of microstructures in the n-type PS layers. Common features for both p-type and n-type PS layers are as follows: the parts which can emit visible photoluminescence are not amorphous, but crystalline, and such parts are composed of nanocrystallites of several nm’s whose orientations are slightly different from Si substrate, and such fine silicon particles absorb much hydrogen atoms near the surfaces. Light emission is strongly dependent on such fine silicon particles. Photoluminescence is due to charge carrier confinement in such three dimensional structure (sponge-like structure). Characteristics of visible light emission from ntype PS can be explained in terms of modification of band structure accompanied by bandgap widening and localized levels in bandstructure. It is also shown that hydrogen and oxygen atoms existing on residual silicon parts play an important role on emission stability.

In this study, we investigated the overpotential of precipitation related to the catalytic activity of electrodes on the initial process of electrodeposition of Co and Co-Ni alloys on polycrystalline Cu substrates. In the case of Co electrodeposition, the surface morphology and the magnetic property change depending on the film thickness, and the relationship with the electrode potential fluctuation was shown. Initially, the deposition potential(−170 mV) of the Cu electrode as a substrate was shown, the electrode potential(Edep) at the Ton of electrodeposition and the deposition potential(−600 mV) of the surface of the electrodeposited Co film after Toff and when the pulse current was completed were shown. No significant change in the electrode potential value was observed when the pulse current was energized. However, in a range of number of pulses up to 5, there was a small fluctuation in the values of Edep and Eimm. In addition, in the Co-Ni alloy electrodeposition, the deposition potential(−280 mV) of the Cu electrode as the substrate exhibited the deposition potential(−615 mV) of the electrodeposited Co-Ni alloy after pulsed current application, the Edep of electrodeposition at the Ton of each pulse and the Eimm at the Toff varied greatly each time the pulse current was applied. From 20 % to less than 90% of the Co content of the thin film was continuously changed, and the value was constant at a pulse number of 100 or more. In any case, it was found that the shape of the substrate had a great influence.

Unidirectionally solidified TiAl alloys were prepared by optically-heated floating zone method at growth rates of 10 to 70 mm/h in flowing argon. The microstructures and tensile properties of these crystal bars were found to depend strongly on the growth rate and alloy composition. TiAl alloys with composition of 47 and 50 at.%Al grown under the condition of 10 mm/h showed Ti3Al(α2)/TiAl(γ) layer structures similar to single crystals. As the growth rate increased, the alloys with 47 and 50 at.%Al compositions showed columnar-grain structures. However, the alloys fabricated under the condition of 10 mm/ h had a layered structure, but the alloy with increased growth rate consisted of γ single phase grains. The alloy with a 53 at.%Al composition showed a γ single phase regardless of the growth rate. Room-temperature tensile tests of these alloys revealed that the columnar-grained material consisting of the layered structure showed a tensile ductility of larger than 4 % and relatively high strength. The high strength is caused by stress concentration at the grain boundaries; this enhances the secondary slip or deformation twinning across the layered structure in the vicinity of the grain boundaries, resulting in the appreciable ductility.

Binary Ti-Al alloys containing 50 to 60 atomic percent aluminum are rapidly solidified by hammer anvil method under an argon atmosphere. Constituent phases in each alloy are identified by X-ray diffractometry and microstructures of the alloys are investigated using a transmission electron microscope. In alloys with aluminum content between 50 and 54 percent, a second phase exists besides TiAl(γ); this second phase is identified as Ti3Al(α2). The α2 phase is observed in two types of morphology. One is as fine lamellar alternating with γ and the other is as a particle. It is concluded that the existence of a metastable phase with the morphologies stated above should arise from a higher quenching rate attained by the hammer anvil method as compared to the conventional roll or splat-quench method. Implications of the above observation are discussed with respect to the phase relations in the Ti-Al binary system; these implications are still controversial in many respects.

Grain morphology, phase stability and mechanical properties in binary Ti-Al alloys containing 43-52 mo1% Al have been investigated. Isothermal forging was used to control the grain sizes of these alloys in the range of 5 to 350 μm. Grain morphology and volume fraction of α2 phase were observed by optical metallography and scanning electron microscopy. Compressive properties were evaluated at room temperature, 1070 K, and 1270 K in an argon atmosphere. Work hardening is significant at room temperature, but it hardly took place at 1070 K and 1270 K because of dynamical recrystallization. The grain morphologies were determined as functions of aluminum content and processing conditions. The transus curve of α and α+γ shifted more to the aluminum-rich side than was the case in McCullough’s phase diagram. Flow stress at room temperature depends strongly on the volume fraction of the α2 phase and the grain size, whereas flow stress at 1070 K is insensitive to the alloy composition or the grain size, and flow stress at 1270 K depends mainly on the grain size. The α2 phase in the alloys does not increase the proof stress at high temperatures. These observations indicate that improvement of both the proof stress at high temperature and the room temperature ductility should be achieved to obtain slightly Ti-rich TiAl base alloys.

Tensile tests and creep tests were carried out at high temperatures on an Al-Al4C3 alloy prepared by mechanical alloying technique. The material contains about 2.0 % carbon and 0.9 % oxygen in mass percent, and the volume fractions of Al4C3 and Al2O3 particles are estimated at 7.4 and 1.4 %, respectively, from the chemical composition. Minimum creep rate decreased steeply near two critical stresses, σcl (the lower critical stress) and σcu (the upper critical stress), with decreasing applied stress at temperatures below 723 K. Instantaneous plastic strain was observed in creep tests above a critical stress, σci, at each test temperature. σcu and σci were fairly close to the 0.2% proof stress obtained by tensile tests at each test temperature. It is thought that σcl and σcu correspond to the microscopic yield stress and the macroscopic yield stress, respectively. The lower critical stress corresponds to the local yield stress needed for dislocations to move in the soft region within subgrains. The creep strain in the low stress range below 723 K arises mainly from the local deformation of the soft region. The upper critical stress is equivalent to the macroscopic yield stress necessary for dislocations within subgrains or in subboundaries; this stress can extensively move beyond subboundaries under a stress above the critical point to yield a macroscopic deformation. At higher temperatures above 773 K, the influence of the diffusional creep increases and the stress exponent of the creep rate decreases.

Ni-C composite films were prepared by co-deposition using a combined technique of plasma CVD and ion beam sputtering deposition. Depending on the deposition conditions, Ni-C thin films manifested three kinds of microstructure: (1) nanocrystallites of non-equilibrium carbide of nickel, (2) amorphous Ni-C film, and (3) granular Ni-C film. The electrical resistivity was also found to vary from about 102 μΩcm for the carbide films to about 104 μΩcm for the amorphous Ni-C films. The Ni-C films deposited at ambient temperatures showed very low TCR values compared with that of metallic nickel film, and all the films showed ohmic characterization, even those in the amorphous state with very high resistivity. The TCR value decreased slightly with increasing of the flow rate of CH4. For the films deposited at 200 oC, TCR decreased with increasing CH4 flow rate; especially, it changed sign from positive to negative at a CH4 flow rate of 0.35 sccm. By increasing the CH4 flow rate, the amorphous component in the film increased; thus, the portion of Ni3C grains separated from each other became larger, and the contribution to electrical conductivity due to thermally activated tunneling became dominant. This also accounts for the sign change of TCR when the filme was deposited at higher flow rate of CH4. The microstructures of the Ni-C films deposited in these ways range from amorphous Ni-C alloy to granular structures with Ni3C nanocrystallites. These films are characterized by high resistivity and low TCR values; the electrical properties can be adjusted over a wide range by controlling the microstructures and compositions of the films.

Ti films were deposited on glass substrates under various preparation conditions in a chamber of two-facing-target type dc sputtering; after deposition, the electric resistivity values were measured using a conventional four-probe method. Crystallographic orientations and microstructures, including the texture and columnar structure, were also investigated for the Ti films. The morphological features, including the columnar structures and surface roughness, are well explained on the basis of Thornton’s zone model. The electric resistivity and the thermal coefficient of the resistivity vary with the sputtering gas pressure. The minimum value of resistivity was around 0.4 Pa for both the 0.5 μm and 3.0 μm thick films; the apparent tendencies are almost the same for the two films, with a small difference in resistivity because of the different film thicknesses. The films deposited at high gas pressures show higher resistivities. The maximum of TCR is also around 0.4 Pa, which is the same as that obtained from the relationship between the resistivity and the gas pressure. The lattice spacing also decreases with increasing sputtering gas pressure for both the 0.5 μm and 3.0 μm thick films. Because they are strongly related to the sputtering gas pressures for Ti films that have a crystallographic anisotropy that is different from cubic symmetry, these changes are well explained on the basis of the film microstructures. It is shown that resistivity measurement can serve as a promising monitor for microstructures in sputtered Ti films.

The high temperature deformation behavior of Ni3Al and Ni3(Al,Mo) single crystals that were oriented near <112> was investigated at low strain rates in the temperature range above the flow stress peak temperature. Three types of behavior were found under the present experimental conditions. In the relatively high strain rate region, the strain rate dependence of the flow stress is small, and the deformation may be controlled by the dislocation glide mainly on the {001} slip plane in both crystals. At low strain rates, the octahedral glide is still active in Ni3Al above the peak temperature, but the active slip system in Ni3(Al,Mo) changes from octahedral glide to cube glide at the peak temperature. These results suggest that the deformation rate controlling mechanism of Ni3Al is viscous glide of dislocations by the <110>{111} slip, whereas that of Ni3(Al,Mo) is a recovery process of dislocation climb in the substructures formed by the <110>{001} slip. The results of TEM observation show that the characteristics of dislocation structures are uniform distribution in Ni3Al and subboundary formation in Ni3(Al,Mo). Activation energies for deformation in Ni3Al and Ni3(Al,Mo) were obtained in the low strain rate region. The values of the activation energy are 360 kJ/mol for Ni3Al and 300 kJ/mol for Ni3(Al,Mo).

Morphology and formation processes of lamellar grain boundaries in titanium rich binary TiAl intermetallics were studied. TiAl alloys containing aluminum content of 44 to 48 at.% were induction-heated to 1723 K followed by helium-gasquenching at various temperatures. For the Ti-44%Al, few lamellae were observed in samples quenched from higher than 1473 K. Although small peaks of beta phase were detected using X-ray diffraction, only the ordered hexagonal phase (α2) with clear APB contrast was observed in TEM observation. For the Ti-48 at.%Al alloy, almost no lamellar structure, and straight grain boundaries were observed in samples quenched from higher than 1623 K. The formation of lamellae along grain boundaries was observed in the sample quenched from 1573 K. The fully lamellar microstructures with serrated boundaries were observed in samples quenched from lower than 1473 K. It was found that the formation of γ platelets took place at higher temperatures in Ti-48 at.%Al than in Ti-44 at.%Al. Although the size of the serration is different, serrated lamellar grain boundaries could be obtained for all alloy compositions employed. The serration appeared to be due to the grain boundary migration induced by precipitation and growth of γ. Differences in transformation characteristics with aluminum content are discussed.

The fatigue strength of a nickel-base superalloy was studied. Stress-controlled fatigue tests were carried out at 700 oC and 5 Hz using triangular wave forms. In this study, two kinds of testing procedures were adopted. One is the conventional tension-zero fatigue test(R = 0). The other was a procedure in which the maximum stress was held at 1000 MPa and the minimum stress was diverse from zero to 1000 MPa at 24 and 700 oC. The results of the fatigue tests at 700 oC indicate that the fracture mechanism changed according to both the mean stress and the stress range. At a higher stress range, γ ' precipitates are sheared by a/2<110> dislocation pairs coupled by APB. Therefore, in a large stress range, the deformation occurred by shearing of γ ' by a/2<110> dislocations, which brought about crystallographic shear fracture. As the stress range was decreased, the fracture mode gradually changed from crystallographic shear fracture to gradual growth of fatigue cracks. At an intermediate stress range, as it became more difficult for a/2<110> dislocation pairs to shear γ ' particles, cracks started to propagate in the matrix, avoiding the harder γ ' particles. High mean stress induced creep deformation, that is, γ ' particles were sheared by {111}<112> slip systems, which led to the formation of stacking faults in the precipitates. Thus, the change in fracture mechanism brought about the inversion of the S-N curves.

Fundamental studies of microstructural changes and high temperature deformation of titanium aluminide (TiAl) were conducted from the view point of the effect of Al content in order to develop the manufacturing process of TiAl. Microstructures in an as cast state consisted mainly of lamellar structure irrespective of Al content. By homogenization at 1473 K, the microstructures of Ti-49Al and Ti-51Al were transformed into an equiaxial structure which was composed of γ-TiAl, while the lamellar structure that was observed in Ti-46Al and Ti-47Al was much more stable. We found that the reduction of Al content suppressed the formation of equiaxial grains and resulted in a microstructure of only a lamellar structure. On Ti-49Al and Ti-51Al, dynamic recrystallization occurred during high temperature deformation, and the microstructure was transformed into a fine equiaxial one, while the microstructures of Ti-46Al and Ti-47Al contained few recrystallized grains and consisted mainly of a deformed lamellar structure. We observed that on the low-Al alloys the lamellar structure under hard mode deformation conditions deformed as kink observed B2-NiAl. High temperature deformation characteristics of TiAl were strongly affected by Al content. An increase of Al content resulted in a decrease of peak stress and activation energy for plastic deformation and an increase of the recrystallization ratio in TiAl.

Aluminum nitride, a compound semiconductor, has a Wurtzite structure; good material properties such as high thermal conductivity, great electric conductivity, high dielectric breakdown strength, a wide energy band gap (6.2eV), a fast elastic wave speed; and excellent in thermal and chemical stability. Furthermore, the thermal expansion coefficient of the aluminum nitride is similar to those of Si and GaAs. Due to these characteristics, aluminum nitride can be applied to electric packaging components, dielectric materials, SAW (surface acoustic wave) devices, and photoelectric devices. In this study, we surveyed the crystallization and preferred orientation of AlN thin films with an X-ray diffractometer. To fabricate the AlN thin film, we used the magnetron sputtering method with N2, NH3 and Ar. According to an increase in the partial pressures of N2 and NH3, Al was nitrified and deposited onto a substrate in a molecular form. When AlN was fabricated with N2, it showed a c-axis orientation and tended toward a high orientation with an increase in the temperature. On the other hand, when AlN was fabricated with NH3, it showed a-axis orientation. This result is coincident with the proposed mechanism. We fabricated AlN thin films with an a-axis orientation by controlling the sputtering electric power, NH3 pressure, deposition speed, and substrate temperature. According to the proposed mechanism, we also fabricated AlN thin films which demonstrated high aaxis and c-axis orientations.