Titanium, which has excellent strength and toughness characteristics, is increasingly used in the aerospace field. Among the titanium alloys used for body parts, more than 80 % are Ti-6Al-4V alloys with a tensile strength of 931 MPa. The spark plasma sintering (SPS) method is used for solidification molding of powder manufactured by the mechanical milling (MM) method, by sintering at low temperature for a short time. This sintering method avoids coarsening of the fine crystal grains or dispersed particles of the MM powder. To improve the mechanical properties of pure titanium without adding alloying elements, stearic acid was added to pure titanium powder as a process control agent (PCA), and MM treatment was performed. The properties of the MM powder and SPS material produced by solidifying the powder were investigated by hardness measurement, X-ray diffraction, density measurement and structure observation. The processing deformation of the pure titanium powder depends on the amount of stearic acid added and the MM treatment time. TiN was also generated in powder treated by MM 8 h with 0.50 g of added stearic acid, and the hardness of the powder was higher than that of Ti-6Al-4V alloy when treated with MM for 8 h. When the MM-treated powder was solidified in the SPS equipment, TiC was formed by the solid phase reaction. The SPS material prepared as a powder treated with MM 8 h by adding 0.50 g of stearic acid also formed TiN and exhibited the highest hardness of Hv1253.

This paper reports the results of an experimental examination using X-rays to test annealing materials for lapped bearing steel (STB2), to confirm the validity of the weighted averaging analysis method. The distribution behavior for the sin diagram and the presence or absence of differences in the peak method, half-value breadth method, and centroid method were investigated. When lapping the annealed bearing steel (STB2) material, a residual stress state with a non-directional steep gradient appeared in the surface layer, and it was found that the weighted averaging analysis method was effective. If there is a steep stress gradient, the sin diagram is curved and the diffraction intensity distribution curve becomes asymmetric, resulting in a difference between the peak method, half-value breadth method, and centroid method. This phenomenon was evident when the stress gradient was more than 2~3 kg/mm2/μm. In this case, if the position of the diffraction line is determined using the centroid method and the weighted averaging analysis method is applied, the stress value on the surface and the stress gradient under the surface can be obtained more accurately. When the stress gradient becomes a problem, since the curvature of the sin diagram appears clearly in the region of sin > 0.5, it is necessary to increase the inclination angle  as much as possible. In the case of a lapping layer, a more accurate value can be obtained by considering  in the weighted averaging analysis method. In an isotropic biaxial residual stress state, the presence or absence of  can be determined as the presence or absence of strain for sin≈0.4.

The most comprehensive and particularly reliable method for non-destructively measuring the residual stress of the surface layer of metals is the sin method. When X-rays were used the relationship of sin measured on the surface layer of the processing metal did not show linearity when the sin method was used. In this case, since the effective penetration depth changes according to the changing direction of the incident X-ray,  becomes a sin function. Since  cannot be used as a constant, the relationship in sin cannot be linear. Therefore, in this paper, the orthogonal function method according to Warren’s diffraction theory and the basic profile of normal distribution were synthesized, and the X-ray diffraction profile was calculated and reviewed when there was a linear strain (stress) gradient on the surface. When there is a strain gradient, the X-ray diffraction profile becomes asymmetric, and as a result, the peak position, the position of half-maximum, and the centroid position show different values. The difference between the peak position and the centroid position appeared more clearly as the strain (stress) gradient became larger, and the basic profile width was smaller. The weighted average strain enables stress analysis when there is a strain (stress) gradient, based on the strain value corresponding to the centroid position of the diffracted X-rays. At the 1/5 max height of X-ray diffraction, the position where the diffracted X-ray is divided into two by drawing a straight line parallel to the background, corresponds approximately to the centroid position.

Magnesium alloy is the lightest practical metal. It has excellent specific strength and recyclability as well as abundant reserves, and is expected to be a next-generation structural metal material following aluminum alloy. This paper investigated the possibility of thin plate fabrication by applying a overheating treatment to the melt drag method, and investigating the surface shape of the thin plate, grain size, grain size distribution, and Vickers hardness. When the overheating treatment was applied to magnesium alloy, the grains were refined, so it is expected that further refinement of grains can be realized if the overheating treatment is applied to the melt drag method. By applying overheating treatment, it was possible to fabricate a thin plate of magnesium alloy using the melt drag method, and a microstructure with a minimum grain size of around 12 μm was obtained. As the overheating treatment temperature increased, void defects increased on the roll surface of the thin plate, and holding time had no effect on the surface shape of the thin plate. The fabricated thin plate showed uniform grain size distribution. When the holding times were 0 and 30 min, the grain size was refined, and the effect of the holding time became smaller as the overheating treatment temperature increased. As the overheating temperature becomes higher, the grain size becomes finer, and the finer the grain size is, the higher the Vickers hardness.

Research is being actively conducted on the continuous thin plate casting method, which is used to manufacture magnesium alloy plate for plastic processing. This study applied a heat transfer solidification analysis method to the melt drag process. The heat transfer coefficient between the molten magnesium alloy metal and the roll in the thin plate manufacturing process using the melt drag method has not been clearly established until now, and the results were used to determine the temperature change. The estimated heat transfer coefficient for a roll speed of 30 m/min was 1.33 × 105 W/m2·K, which was very large compared to the heat transfer coefficient used in the solidification analysis of general aluminum castings. The heat transfer coefficient between the molten metal and the roll estimated in the range of the roll speed of 5 to 90 m/min was 1.42 × 105 to 8.95 × 104 W/m2·K. The cooling rate was calculated using a method based on the results of deriving the temperature change of the molten metal and the roll, using the estimated heat transfer coefficient. The DAS was estimated from the relationship between the cooling rate and DAS, and compared with the experimental value. When the magnesium alloy is manufactured by the melt drag method, the cooling rate of the thin plate is in the range of about 1.4 × 103 to 1.0 × 104 K/s.

AZ31 magnesium alloy was used to manufacture a thin plate using a melt drag method. The effects of roll speed, molten metal temperature, and molten metal height, which are the basic factors of the melt drag method, on the surface shape, the thickness of the thin plate, Vickers hardness, and microstructure of the thin plate were investigated. It was possible to manufacture AZ31 magnesium alloy thin plate at the roll speed range of 1 to 90 m/min. The thickness of the thin plate, manufactured while changing only the roll speed, was about 1.8 to 8.8 mm. The shape of the solidified roll surface was affected by two conditions, the roll speed and the molten metal height, and the Vickers hardness of the manufactured magnesium alloy thin plate value ranged from Hv38~Hv60. The microstructure of the thin plate produced by this process was an equiaxed crystal and showed a uniform grain size distribution. The grain size was greatly affected by the contact state between the molten metal and the solidification roll, and the amount of reactive solids and liquids scraped at the same time as the thin plate. The average grain size of the thin plate fabricated in the range of these experimental conditions changed to about 50-300 μm.

Aluminum nitride having a dense hexagonal structure is used as a high-temperature material because of its excellent heat resistance and high mechanical strength; its excellent piezoelectric properties are also attracting attention. The structure and residual stress of AlN thin films formed on glass substrate using TFT sputtering system are examined by XRD. The deposition conditions are nitrogen gas pressures of 1 × 102, 6 × 103, and 3 × 103, substrate temperature of 523 K, and sputtering time of 120 min. The structure of the AlN thin film is columnar, having a c-axis, i.e., a <00·1> orientation, which is the normal direction of the glass substrate. An X-ray stress measurement method for crystalline thin films with orientation properties such as columnar structure is proposed and applied to the residual stress measurement of AlN thin films with orientation <00·1>. Strength of diffraction lines other than 00·2 diffraction is very weak. As a result of stress measurement using AlN powder sample as a comparative standard sample, tensile residual stress is obtained when the nitrogen gas pressure is low, but the gas pressure increases as the residual stress is shifts toward compression. At low gas pressure, the unit cell expands due to the incorporation of excess nitrogen atoms.

To improve the shortcomings and expand the advantages of the single-roll melt drag method, which is a type of continuous strip casting method, the melt drag method with a molding belt is applied to AZ31 magnesium alloy. By attaching the forming belt to the melt drag method, the cooling condition of the thin plate is improved, making it possible to manufacture thin plates even at high roll speed of 100 m/min or more. In addition, it is very effective for continuous production of thin plates to suppress oxidation of the molten metal on the roll contact surface by selecting the protective gas. As a result of investigating the relationship between the contact time between the molten metal and the roll and the thickness of the sheet, it is possible to estimate the thickness of the sheet from the experimental conditions. The relationship between the thin plate thickness and the grain size is one in which the thinner the thin plate is, the faster the cooling rate of the thin plate is, resulting in finer grain size. The contact state between the molten metal and the roll greatly affects the grain size, and the minimum average grain size is 72 μm. The thin plate produced using this experimental equipment can be rolled, and the rolled sample has no large cracks. The tensile test results show a tensile strength of 303 MPa.

An investigation is performed to clarify the manufacturing conditions of pure magnesium and AZ31 magnesium alloy thin plate using the melt drag method. By the melt drag method, suitable for magnesium molten metal, pure magnesium can be produced as a continuous thin plate with a thickness of 1.4 mm to 2.4 mm in the range of 5 m/min to 20 m/min of roll speed, and the width of the thin plate to the nozzle outlet width. AZ31 magnesium alloy is able to produce a continuous sheet of thickness in the range of 5 m/min to 30 m/min in roll circumferential speed, with a thickness of 0.6 mm to 1.6 mm and a width of the sheet matching the nozzle outlet width. In the magnesium melt drag method, the faster the circumferential speed of the roll, the shorter the contact time between the molten metal and the roll, and it is found that the thickness of the produced thin plate becomes thinner. The effect of the circumferential roll speed on the thickness of the thin plate is evident in the low roll circumferential region, where the circumferential speed is 30 m/min or less. The AZ31 thin plate manufactured by the melt drag method has a finer grain size as the thickness of the thin plate decreases, but it is currently judged that this is not the effect of cooling by the roll.

Al-Cr-Si ternary quench ribbons are fabricated using a single roll method and investigated for their structural and thermal properties. In particular, the sinterability is examined by pulse current sintering to obtain the following results. The Al74Cr20Si6 composition becomes a quasicrystalline single phase; by reducing the amount of Cr, it becomes a twophase mixed structure of Al phase and quasicrystalline phase. As a result of sintering of Al74Cr20Si6, Al77Cr13Si10 and Al90Cr6Si4 compositions, the sintering density is increased with the large amount of Al phase; the sintering density is the highest in Al90Cr6Si4 composition. In addition, as a result of investigating the effects of sintering temperature and pressurization on the sintered density of Al90Cr6Si4, a sintered compact of 99% or more at 513 K and 500 MPa is produced. In particular, since the Al-Cr-Si ternary crystal is more thermally stable than the Al-Cr binary quaternary crystal, it is possible to increase the sintering temperature by about 100 K. Therefore, using an alloy of Al90Cr6Si4 composition, a sintered compact having a sintered density of 99 % or more at 613 K and 250 MPa can be manufactured. It is possible to increase the sintering temperature by using the alloy system as a ternary system. As a result, it is possible to produce a sintered body with higher density than that possible using the binary system, and at half the pressure compared with the conventional Al-Cr binary system.

In this study, using the plasma spray method, tensile and compression fatigue tests are performed in saline solution to examine the effect of Ti undercoat on corrosion fatigue behavior of alumina-coated specimens. The alumina-coated material using Ti in the undercoat shows better corrosion fatigue strength than the base material in the entire stress amplitude range. Fatigue cracking of UT specimens occurs in the recess formed by grit-blasting treatment and progresses toward the base metal. Subsequently, the undercoat is destroyed at a stage where the deformation of the undercoat cannot follow the crack opening displacement. The residual stress of the UT specimen has a tensile residual stress up to about 100 μm below the surface of the base material; however, when the depth exceeds 100 μm, the residual stress becomes a compressive residual stress. In addition, the inside of the spray coating film is compressive residual stress, which contributes to improving the fatigue strength characteristics. A hardened layer due to grit-blasting treatment is formed near the surface of the UT specimen, contributing to the improvement of the fatigue strength characteristics. Since the natural potential of Ti spray coating film is slightly higher than that of the base material, it exhibits excellent corrosion resistance; however, when physiological saline intrudes, a galvanic battery is formed and the base material corrodes preferentially.

In this study, high temperature wetting analysis and AZ80/Ti interfacial structure observation are performed for the mixture of AZ80 and Ti, and the effect of Al on wetting in Mg alloy is examined. Both molten AZ80 and pure Mg have excellent wettability because the wet angle between molten droplets and the Ti substrate is about 10° from initial contact. Wetting angle decreases with time, and wetting phenomenon continues between droplets and substrate; the change in wetting angle does not show a significant difference when comparing AZ80-Ti and Mg-Ti. As a result of XRD of the lower surface of the AZ80-Ti sample, in addition to the Ti peak of the substrate, the peak of TiAl3, which is a Ti-Al intermetallic compound, is confirmed, and TiAl3 is generated in the Al enrichment region of the Ti substrate surface. EDS analysis is performed on the droplet tip portion of the sample section in which pure Mg droplets are dropped on the Ti substrate. Concentration of oxygen by the natural oxide film is not confirmed on the Ti surface, but oxygen is distributed at the tip of the droplet on the Mg side. Molten AZ80 and Ti-based compound phases are produced by thickening of Al in the vicinity of Ti after wetting is completed, and Al in the Mg alloy does not affect the wetting. The driving force of wetting progression is a thermite reaction that occurs between Mg and TiO2, and then Al in AZ80 thickens on the Ti substrate interface to form an intermetallic compound.

A variety of composite powders having different aluminum and carbon contents are prepared using various organic solvents having different amounts of carbon atoms in unit volume as ball milling agents for titanium and aluminum ball milling. The effects of substrate temperature and post-heat treatment on the texture and hardness of the coating are investigated by spraying with this reduced pressure plasma spray. The aluminum part of the composite powder evaporates during spraying, so that the film aluminum content is 30.9 mass%~37.4 mass% and the carbon content is 0.64 mass%~1.69 mass%. The main constituent phase of the coating formed on the water-cooled substrate is a non-planar α2 phase, obtained by supersaturated carbon regardless of the alloy composition. When these films are heat-treated at 1123 K, the main constituent phase becomes  phase, and fine Ti2AlC precipitates to increase the film hardness. However, when heat treatment is performed at a higher temperature, the hardness is lowered. The main constitutional phase of the coating formed on the preheated substrate is an equilibrium gamma phase, and fine Ti2AlC precipitates. The hardness of this coating is much higher than the hardness of the coating in the sprayed state formed on the water-cooled substrate. When hot pressing is applied to the coating, the porosity decreases but hardness also decreases because Ti2AlC grows. The amount of Ti2AlC in the hot-pressed film is 4.9 vol% to 15.3 vol%, depending on the carbon content of the film.

In this study, factors considered to be causes of promotion of densification of sintered pellets identified during phase change are reviewed. As a result, conclusions shown below are obtained for each factor. In order for MA powder to soften, a temperature of 1,000 K or higher is required. In order to confirm the temporary increase in density throughout the sintered pellet, the temperature rise due to heat during phase change was found not to have a significant effect. While examining the thermal expansion using the compressed powder, which stopped densification at a temperature below the MA powder itself, and the phase change temperature, no shrinkage phenomenon contributing to the promotion of densification is observed. The two types of powder made of Ti-silicide through heat treatment are densified only in the high temperature region of 1,000 K or more; it can be estimated that this is the effect of fine grain superplasticity. In the densification of the amorphous powder, the dependence of sintering pressure and the rate of temperature increase are shown. It is thought that the specific densification behavior identified during the phase change of the Ti-37.5 mol.%Si composition MA powder reviewed in this study is the result of the acceleration of the powder deformation by the phase change from non-equilibrium phase to equilibrium phase.

The composition of martensite transformation in NiAl alloy is determined using pure nickel and aluminum powder by vacuum hot press powder metallurgy, which is a composition of martensitic transformation, and the characteristics of martensitic transformation and microstructure of sintered NiAl alloys are investigated. The produced sintered alloys are presintered and hot pressed in vacuum; after homogenizing heat treatment at 1,273 K for 86.4 ks, they are water-cooled to produce NiAl sintered alloys having relative density of 99 % or more. As a result of observations of the microstructure of the sintered NiAl alloy specimens quenched in ice water after homogenization treatment at 1,273 K, it is found that specimens of all compositions consisted of two phases and voids. In addition, it is found that martensite transformation did not occur because surface fluctuation shapes did not appear inside the crystal grains with quenching at 1,273 K. As a result of examining the relationship between the density and composition after martensitic transformation of the sintered alloys, the density after transformation is found to have increased by about 1 % compared to before the transformation. As a result of examining the relationship between the hardness (Hv) at room temperature and the composition of the matrix phase and the martensite phase, the hardness of the martensite phase is found to be smaller than that of the matrix phase. As a result of examining the relationship between the temperature at which the shape recovery is completed by heating and the composition, the shape recovery temperature is found to decrease almost linearly as the Al concentration increases, and the gradient is about -160 K/ at% Al. After quenching the sintered NiAl alloys of the 37 at%Al into martensite, specimens fractured by three-point bending at room temperature are observed by SEM and, as a result, some grain boundary fractures are observed on the fracture surface, and mainly intergranular cleavage fractures.

In order to observe the microstructure and morphology of porous titanium -oxide thin film, deposition is performed under a higher Ar gas pressure than is used in the general titanium thin film production method. Black titanium thin film is deposited on stainless steel wire and Cu thin plate at a pressure of about 12 Pa, but lustrous thin film is deposited at lower pressure. The black titanium thin film has a larger apparent thickness than that of the glossy thin film. As a result of scanning electron microscope observation, it is seen that the black thin film has an extremely porous structure and consists of a separated column with periodic step differences on the sides. In this configuration, due to the shadowing effect, the nuclei formed on the substrate periodically grow to form a step. The surface area of the black thin film on the Cu thin plate changes with the bias potential. It has been found that the bias of the small negative is effective in increasing the surface area of the black titanium thin film. These results suggest that porous titanium-oxide thin film can be fabricated by applying the appropriate oxidation process to black titanium thin film composed of separated columns.

In order to develop a process for manufacturing a composite structure of an intermetallic compound foam and a hollow material, the firing and pore form of the Al-Ni precursor in a steel pipe are investigated. When the Al-Ni precursor is foamed in a hollow pipe, if the temperature distribution inside the precursor is uneven, the pore shape distribution becomes uneven. In free foaming, no anisotropy is observed in the foaming direction and the pore shape is isotropic. However, in the hollow pipe, the pipe expands in the pipe axis direction and fills the pipe. The interfacial adhesion between Al3Ni foam and steel pipe is excellent, and interfacial pore and reaction layer are not observed by SEM. In free foaming, the porosity is 90 %, but it decreases to about 80 % in the foam in the pipe. In the pipe foaming, most of the pore shape appears elongated in the pipe direction in the vicinity of the pipe, and this tendency is more remarkable when the inside pipe diameter is small. It can be seen that the pore size of the foam sample in the pipe is larger than that of free foam, because coarse pores remain after solidification of the foam because the shape of the foam is supported by the pipe. The vertical/horizontal length ratio expands along the pipe axis direction by foaming in the pipe, and therefore circularity is reduced.

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.

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.