Microstructure and hardness of Mg-based composites reinforced with Mg2Si particles

Magnesium powders were mechanically alloyed with SiO2 powder particles having different particle sizes using high-energy ball milling techniques under Ar atmosphere for 1 h. The powders were consolidated with cold pressing under 560 Mpa. They were then sintered at 550℃ for 45 min under Ar atmosphere. The composites obtained on the Mg-SiO2 system were investigated using the Archimedes principle, a differential scanning calorimeter, X-ray diffraction, optic microscopy, and scanning electron microscopy. For the mechanically alloyed powders, the solid-state reaction of the synthesis of Mg2Si and MgO progressed further during sintering of the materials. The results showed that the strengthening mechanisms were dependent on dispersion hardening of fine Mg2Si and MgO particulates dispersed homogeneously in the matrix.     

Pressure-composition-isotherm behavior of nano-/amorphous Mg<Subscript>2</Subscript>NiH<Subscript>x</Subscript>

It has recently been shown that the hydriding properties of the nanocrystalline metal hydrides are far superior to those of the polycrystalline ones. Especially in the case of the Mg-based hydrogen storage alloys, nanostructural modifications have been studied for the purpose of improving their hydrogenation kinetics. In previous studies, I reported on the successful fabrication of Mg₂NiH_x from Mg and Ni chips with hydrogen induced mechanical alloying (HIMA). Observation of the microstructure showed that the synthesized particles (processed with a 66:1 ball to chips mass ratio and 96 hr HIMA) are composed of amorphous and nanocrystalline composite phases with a grain size of less than 10 nm. The aim of the present work was to examine the hydriding/dehydriding behavior of nanocrystalline metal hydrides using a Sieverts type automatic pressure-composition-isotherm (PCI) apparatus at 393, 423, 453, 483, 513 and 543 K. The specimen was characterized by X-ray diffraction after PCI measurement. The influence of hydrogenation behavior on the phase transition of nano-/amorphous Mg₂Ni is a key factor in commercial application. The particles synthesized at 66:1 BCR and 96 hr HIMA revealed a good hydrogen capacity of 2.25 mass% at 483 K.     

Studies on Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/ZrO<Subscript>2</Subscript>/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> high K gate dielectrics applied in a fully depleted SOI MOSFET

Al₂O₃/ZrO₂/Al₂O₃ gate stacks were prepared on ultrathin SOI (Silicon on insulator) substrates by ultrahigh vacuum electron beam evaporation and post-annealed in N₂ at 450°C for 30 min. Three clear nanolaminate layered structure of Al₂O₃(2.1 nm)/ZrO₂(3.5 nm)/Al₂O₃(2.3 nm) was observed with a high-resolution cross-sectional transmission electron microscope (HR-XTEM). High frequency capacitance voltage (C-V) characteristics of a fully depleted (FD) SOI MOS capacitor at 1 and 5 MHz were studied. The minority carriers determine the high frequency C-V properties, which is opposite to the case of bulk MOS capacitors. The series resistance of the SOI substrate is found to be the determinant factor of the high frequency characteristics of FD SOI MOS capacitors. This article is based on a presentation in “The 7th Korea-China Workshop on Advanced Materials” organized by the Korea-China Advanced Materials Cooperation Center and the China-Korea Advanced Materials Cooperation Center, held at Ramada Plaza Jeju Hotel, Jeju Island, Korea on August 24≈27, 2003.     

Structure and electric property comparison between Ge nanoclusters embedded in Al<Subscript>2</Subscript>O<Subscript>3</Subscript> and Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/ZrO<Subscript>2</Subscript>

Metal-insulator-semiconductor (MIS) structures containing Ge nanocrystals embedded in both Al₂O₃ and ZrO₂/Al₂O₃ are fabricated by an ultra-high vacuum electron-beam evaporation method. Secondary ion mass spectroscopy (SIMS) results indicate that Ge embedded in Al₂O₃ diffuses towards the surface of the Al₂O₃ layer after annealing at 800°C in N₂ ambient for 30 min. Ge embedded in ZrO₂/Al₂O₃ is stable, thus inducing less leakage current. Capacitance voltage studies indicate that annealing can effectively passivate the negatively charged trapping centers. Memory effect of the Ge nanoclusters is verified by hysteresis in the C-V curves in the Al₂O₃/Ge+Al₂O₃/Al₂O₃ and ZrO₂/Ge+Al₂O₃/Al₂O₃ samples. This article is based on a presentation in “The 7th Korea-China Workshop On Advanced Materials” organized by the Korea-China Advanced Materials Cooperation Center and the China-Korea Advanced Materials Cooperation Center, held at Ramada Plaza Jeju Hotel, Jeju Island, Korea on August 24–27, 2003.     

Effect of Al<Subscript>2</Subscript>O<Subscript>3</Subscript> particles on the microstructure and sliding wear of 7075 Al alloy manufactured by squeeze casting method

Aluminum (Al) alloy 7075 reinforced with Al₂O₃ particles was prepared using the stir casting method. The microstructure of the cast composites showed some degree of porosity and sites of Al₂O₃ particle clustering, especially at high-volume fractions of Al₂O₃ particles. Different squeeze pressures (25 and 50 MPa) were applied to the cast composite during solidification to reduce porosity and particle clusters. Microstructure examinations of the squeeze cast composites showed remarkable grain refining compared with that of the matrix alloy. As the volume fraction of particles and applied squeeze pressure increased, the hardness linearly increased. This increase was related to the modified structure and the decrease in the porosity. The effect of particle volume fraction and squeeze pressure on the dry-sliding wear of the composites was studied. Experiments were performed at 10, 30, and 50 N with a sliding speed of 1 m/s using a pin-on-ring apparatus. Increasing the particle volume fraction and squeeze pressure improved the wear resistance of the composite compared with that of the monolithic alloy, because the Al₂O₃ particles acted as load-bearing constituents. Also, these results can be attributed to the fact that the application of squeeze pressure during solidification led to a reduction in the porosity, and an increase in the solidification rate, leading to a finer structure. Moreover, the application of squeeze pressure improved the interface strength between the matrix and Al₂O₃ particles by elimination of the porosity at the interface, thereby providing better mechanical locking.     

Effect of Mn on the mechanical properties and microstructure of reaction sintered Mo<Subscript>2</Subscript>NiB<Subscript>2</Subscript> boride-based cermets

This paper focused on the effects of Mn addition from 0 to 10wt% on the mechanical properties and microstructure of V added Mo₂NiB₂ based model cermets. Transverse rupture strength of the cermets increased with increasing Mn content and showed a maximum value of 3.5 GPa at 2.5 wt.%Mn, and then decreased with further increasing Mn content. Hardness increased monotonically from 86.4R_A up to 10wt%Mn. The high TRS at 2.5 wt.%Mn was attributed to size refinement and homogeneous distribution of Mo₂NiB₂ complex boride resulting from Mn addition. This article is based on a presentation made in the symposium “The 3rd KIM-JIM Joint Symposium on Advanced Powder Materials”, held at Korea University, Seoul, Korea, October 26–27, 2001 under auspices of The Korean Institute of Metals and Materials and The Japan Institute of Metals.     

Preparation and characterization of nanostructured Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript> and Sn<Subscript>0.5</Subscript>-Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript>

Nanostructured Bi₂Se₃ and Sn_0.5-Bi₂Se₃ were successfully synthesized by hydrothermal coreduction from SnCl₂·H₂O and the oxides of Bi and Se. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscope (FESEM). Bi₂Se₃ powders obtained at 180°C and 150°C consist of hexagonal flakes of 50–150 nm in side length and nanorods of 30–100 nm in diameter and more than 1 μm in length. The product obtained at 120°C is composed of thin irregular nanosheets with a size of 100–200 nm and several nanometers in thickness. The major phase of Sn_0.5-Bi₂Se₃ synthesized at 180°C is similar to that of Bi₂Se₃. Sn_0.5-Bi₂Se₃ powders are primarily nanorod structures, but small amount of powders demonstrate irregular morphologies.     

Structure and magnetic properties of mechanically alloyed Tb0.2Pr0.8（Fe0.4Co0.6）1.93 and magnetostriction of its epoxy composite

The C15 Laves phase with composition Tb_0.2Pr_0.8(Fe_0.4Co_0.6)_1.93 was synthesized by mechanical alloying (MA) and subsequent annealing process. The structure and magnetic properties of Tb_0.2Pr_0.8(Fe_0.4Co_0.6)_1.93 were investigated by means of X-ray diffraction (XRD), a vibrating sample magnetometer, and a standard strain technique. The effect of annealing on the structure and magnetic properties was studied. The analysis of XRD shows that the high Pr-content Tb_0.2Pr_0.8(Fe_0.4Co_0.6)_1.93 alloy with the single phase of MgCu₂-type structure can be successfully synthesized by MA method. The sample annealed at 450°C is found to have a coercivity of 196 kA/m at room temperature. An epoxy/Tb_0.2Pr_0.8(Fe_0.4Co_0.6)_1.93 composite was produced by a cold isostatic pressing technique. A large magnetostriction of 400 ppm, at an applied magnetic field of 800 kA/m, was found for the composite. The epoxy-bonded Tb_0.2Pr_0.8(Fe_0.4Co_0.6)_1.93 composite combines a high magnetostriction with a significant coercivity, which is a promising magnetostrictive material.     

Tensile and wear properties of rolled Al5Mg-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> or C particulate composites

Al5Mg alloy matrix composites reinforced with different percentages of Al₂O₃ (60 μm) or C (90 μm) particulates were prepared by the vortex method. The composites were then subjected to hot or cold rolling with different reduction ratios. The microstructures of the rolled composites revealed that the matrix grains moved around the particulate causing deformation. By continuing deformation, the particulates rearranged themselves in the matrix, leading to lensoid distortion. It was found that the addition of Al₂O₃ or C particulates increased the 0.2% proof stress and reduced both the tensile strength and ductility, compared with the monolithic alloy. Scanning electron microscopy (SEM) fractographic examinations showed that the composites reinforced with Al₂O₃ particulates failed through particulate fracture and matrix ligament rupture. However, the failure of the composites reinforced with C particulates was through particulate decohesion, followed by ductile failure of the matrix. Abrasive wear results showed that the wear rate of the Al5Mg alloy decreased with the addition of C particulates. However, increasing the volume fraction of C particulates did not have a prominent effect on the wear rate. The composites reinforced with Al₂O₃ particulates exhibited a higher wear rate than that of the unreinforced alloy. Furthermore, addition of both C and Al₂O₃ particulates into the Al5Mg matrix alloy did not significantly improve the wear resistance. For all composites studied in this work, hot or cold rolling had a marginal effect on the wear results.     

Cold spray of SiC and Al<Subscript>2</Subscript>O<Subscript>3</Subscript> with soft metal incorporation: A technical contribution

Al + SiC, Al + Al₂O₃ composites as well as pure Al, SiC, and Al₂O₃ coatings were prepared on Si substrates by the cold gas dynamic spray process (CGDS or cold spray). The powder composition of metal (Al) and ceramic (SiC, Al₂O₃) was varied into 1:1 and 10:1 wt.%, respectively. The propellant gas was air heated up to 330 °C and the gas pressure was fixed at 0.7 MPa. SiC and Al₂O₃ have been successfully sprayed producing coatings with more than 50 μm in thickness with the incorporation of Al as a binder. Also, hard ceramic particles showed peening effects on the coating surfaces. In the case of pure Al metal coating, there was no crater formation on hard Si substrates. However, when Al mixed with SiC and Al₂O₃, craters were observed and their quantities and sizes depended on the composition, aggregation and size of raw materials.     

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.     

Corrosive wear behavior of 7075 aluminum alloy and its composite containing Al<Subscript>2</Subscript>O<Subscript>3</Subscript> particles

Corrosive wear behavior of 7075 aluminum alloy and a composite containing 0.10 volume fraction of alumina particles (VFAP) has been evaluated. Transient current (TC) generated as a result of impacting a rotating cylindrical electrode immersed in a 0.1M NaCl solution with a Vickers diamond hardness indenter has been used to measure the corrosive wear response. Age hardenable 7075 alloy shows TC values that are sensitive to prior solutionizing time. The effect of alumina particles in a 7075 aluminum alloy matrix has been studied by comparing the TC values of a monolith along with composites under almost identical experimental conditions. The role of microstructural features associated with composites, such as dislocations generated after solutionizing treatment and during the corrosive wear process, has been observed with the help of near surface microstructures through transmission electron microscopy (TEM). Deformation induced dislocations, as well as those that are due to differences in the coefficient of thermal expansion (CTE) values between the particles and the matrix during solutionizing, have been attributed to the experimentally observed TC values. They may also be affected by the aging response of the monolith and composites, depending on solutionizing time.     

Properties and consolidation of nanostructured Ce<Subscript>0.8</Subscript>Gd<Subscript>0.2</Subscript>O<Subscript>1.9</Subscript> by pulsed-current-activated sintering

Dense nanophase Ce_0.8Gd_0.2O_1.9 was sintered by a pulsed-current-activated sintering method within 10 min from Ce_0.8Gd_0.2O_1.9 nanopowder made using the co-precipitation method. Sintering was accomplished under the combined effects of a pulsed current and mechanical pressure. Highly dense Ce_0.8Gd_0.2O_1.9 with a relative density of up to 96.5% was produced under the simultaneous application of 80 MPa of pressure and a pulsed current. The ionic conductivities and mechanical properties of the Ce_0.8Gd_0.2O_1.9 were investigated.     

Fabrication of Ti<Subscript>3</Subscript>AlC<Subscript>2</Subscript> ceramic material by mechanical alloying

Ti₃AlC₂ has the properties of ceramics and metals. These excellent properties indicate that Ti₃AlC₂ is a very promising material to extensive applications. Ti₃AlC₂ ceramic material was prepared by mechanical alloying. The effects of milling time and sintering temperature on the fracture, microstructure and mechanical properties of Ti₃AlC₂ ceramic material were analyzed by laser particle analyzer, X-ray diffraction, and scanning electron microscopy. The experimental results showed that Ti₃AlC₂ had the best comprehensive properties after the composite powder was milled for 3 h and sintered at 1630°C for 2 h. The relative density, bending strength, and hardness of the sample reached 92.23%, 345.2 MPa, and HRA 34.1, respectively. The fracture surface indicated that the fracture of the material belonged to ductile rapture.     

HVOF-Sprayed Coatings Engineered from Mixtures of Nanostructured and Submicron Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiO<Subscript>2</Subscript> Powders: An Enhanced Wear Performance

In previous studies, it has been demonstrated that nanostructured Al₂O₃-13 wt.%TiO₂ coatings deposited via air plasma spray (APS) exhibit higher wear resistance when compared to that of conventional coatings. This study aimed to verify if high-velocity oxy-fuel (HVOF)-sprayed Al₂O₃-13 wt.%TiO₂ coatings produced using hybrid (nano + submicron) powders could improve even further the already recognized good wear properties of the APS nanostructured coatings. According to the abrasion test results (ASTM G 64), there was an improvement in wear performance by a factor of 8 for the HVOF-sprayed hybrid coating as compared to the best performing APS conventional coating. When comparing both hybrid and conventional HVOF-sprayed coatings, there was an improvement in wear performance by a factor of 4 when using the hybrid material. The results show a significant antiwear improvement provided by the hybrid material. Scanning electron microscopy (SEM) at low/high magnifications showed the distinctive microstructure of the HVOF-sprayed hybrid coating, which helps to explain its excellent wear performance. This article is an invited paper selected from presentations at the 2007 International Thermal Spray Conference and has been expanded from the original presentation. It is simultaneously published in Global Coating Solutions, Proceedings of the 2007 International Thermal Spray Conference, Beijing, China, May 14-16, 2007, Basil R. Marple, Margaret M. Hyland, Yuk-Chiu Lau, Chang-Jiu Li, Rogerio S. Lima, and Ghislain Montavon, Ed., ASM International, Materials Park, OH, 2007.     

Effect of a surface treatment for LiNi<Subscript>1/3</Subscript>Co<Subscript>1/3</Subscript>Mn<Subscript>1/3</Subscript>O<Subscript>2</Subscript> cathode material in lithium secondary batteries

LiNi_1/3Co_1/3Mn_1/3O₂ cathode material was surface-treated to improve its electrochemical performance. Al₂O₃ nanoparticles were coated onto the surface of LiNi_1/3Co_1/3Mn_1/3O₂ powder using a sol-gel method. The as-prepared Al₂O₃ nano-particle was identified as the cubic structure of Al₂O₃. XRD showed that the LiNi_1/3Co_1/3Mn_1/3O₂ structure was not affected by the Al₂O₃ coating. With a coating of 3 wt.% Al₂O₃ on LiNi_1/3Co_1/3Mn_1/3O₂, the cyclic-life performance and rate capability were improved. However, heavier coatings (5 wt.%) on LiNi_1/3Co_1/3Mn_1/3O₂ resulted in a considerable decrease of the discharge capacity and rate capability. The thermal stability of LiNi_1/3Co_1/3Mn_1/3O₂ materials was greatly improved by the 3 wt.% Al₂O₃ coating.     

Electromagnetic wave absorbing properties of Fe<Subscript>73</Subscript>Si<Subscript>16</Subscript>B<Subscript>7</Subscript>Nb<Subscript>3</Subscript>Cu<Subscript>1</Subscript> base P/M sheets mixed with dielectric fine particles

Fe-based nanocrystalline powder sheets with dielectric TiO₂ powder additives were investigated to improve the characteristics of electromagnetic (EM) wave absorption. The amorphous ribbons of Fe₇₃Si₁₆B₇Nb₃Cu₁ (at.%) alloys were prepared by a planar flow casting (PFC) process, and the ribbons were pulverized using an attrition mill. Fe-based flake powder crystallized at 550°C for 1h was mixed with a nano-sized and a micro-sized TiO₂ powder. The powder mixtures were then tape-cast with binders to become EM wave-absorbing sheets. The absorbing properties of the fabricated sheet sample, such as complex permittivity and permeability, were measured by a network analyzer. The properties of EM wave absorption improved with the increase of TiO₂ powder in the mixture. The mixture with micro-sized TiO₂ powder was a little more effective in causing power loss of EM waves than the mixture with nano-sized TiO₂ powder.     

Effects of defects generated in ALD TiO<Subscript>2</Subscript> films on electrical properties and interfacial reaction in TiO<Subscript>2</Subscript>/SiO<Subscript>2</Subscript>/Si system upon annealing in vacuum

Thin TiO₂ layers grown at 130°C on SiO₂-coated Si substrates by atomic layer deposition (ALD) using TTIP and H₂O as precursors were annealed, and the effects of the annealing temperature on the resulting electrical properties of TiO₂ and the interface properties between a Pt electrode and TiO₂ were examined using transmission line model (TLM) structures. The as-deposited TiO₂ thin film had an amorphous structure with OH groups and a high resistivity of 6×10³Ω-cm. Vacuum annealing at 700 °C transformed the amorphous film into an anatase structure and reduced its resistivity to 0.04Ω-cm. In addition, the vacuum-annealing of the TiO₂/SiO₂ structure at 700°C produced free silicon at the TiO₂-SiO₂ interface as a result of the reaction between the Ti interstitials and SiO₂. The SiO₂ formed on the TiO₂ surface caused a Schottky contact, which was characterized by the TLM method. The use of the TLM method enabled the accurate measurement of the resistivity of the vacuum-annealed TiO₂ films and the characterization of the Schottky contacts of the metal electrode to the TiO₂.     

Interdiffusion in <Emphasis Type="Italic">L</Emphasis>1<Subscript>2</Subscript>-Ni<Subscript>3</Subscript>Al Alloyed with Re

Ternary interdiffusion in L1₂-Ni₃Al with ternary alloying addition of Re was investigated at 1473 K using solid-to-solid diffusion couples. Interdiffusion flux of Ni, Al, and Re were directly calculated from experimental concentration profiles and integrated for the determination of average ternary interdiffusion coefficients. The magnitude of main interdiffusion coefficients and was determined to be much larger than that of the main interdiffusion coefficient A moderate tendency for Re to substitute for Al sites was reflected by its influence on interdiffusion of Al, quantified by large and positive coefficients. Similar trends were observed from ternary interdiffusion coefficients determined by Boltzmann-Matano analysis. Profiles of concentrations and interdiffusion fluxes were also examined to estimate binary interdiffusion coefficients in Ni₃Al, and tracer diffusion coefficients of Re (5.4 × 10⁻¹⁶ ± 2.3 × 10⁻¹⁶ m²/s) in Ni₃Al.