Wetting of grain boundaries in Al by the solid Al<Subscript>3</Subscript>Mg<Subscript>2</Subscript> phase

The microstructure of binary Al_100−x –Mg _x (x = 10, 15, 18 and 25 wt%) alloys after long anneals (600–4000 h) was studied between 210 and 440 °C. The transition from incomplete to complete wetting of Al/Al grain boundaries (GBs) by the second solid phase Al₃Mg₂ has been observed. The portion of completely wetted GBs increases with increasing temperature beginning from T _wsmin = 220 °C. Above T _wsmax = 410 °C all Al/Al GBs are completely wetted by the Al₃Mg₂ phase.     

Precipitation in cold-rolled Al–Sc–Zr and Al–Mn–Sc–Zr alloys prepared by powder metallurgy

The effects of cold-rolling on thermal, mechanical and electrical properties, microstructure and recrystallization behaviour of the AlScZr and AlMnScZr alloys prepared by powder metallurgy were studied. The powder was produced by atomising in argon with 1% oxygen and then consolidated by hot extrusion at 350 °C. The electrical resistometry and microhardness together with differential scanning calorimetry measurements were compared with microstructure development observed by transmission and scanning electron microscopy, X-ray diffraction and electron backscatter diffraction. Fine (sub)grain structure developed and fine coherent Al₃Sc and/or Al₃(Sc,Zr) particles precipitated during extrusion at 350 °C in the alloys studied. Additional precipitation of the Al₃Sc and/or Al₃(Sc,Zr) particles and/or their coarsening was slightly facilitated by the previous cold rolling. The presence of Sc,Zr-containing particles has a significant antirecrystallization effect that prevents recrystallization at temperatures minimally up to 420 °C. The precipitation of the Al₆Mn- and/or Al₆(Mn,Fe) particles of a size ~ 1.0 μm at subgrain boundaries has also an essential antirecrystallization effect and totally suppresses recrystallization during 32 h long annealing at 550 °C. The texture development of the alloys seems to be affected by high solid solution strengthening by Mn. The precipitation of the Mn-containing alloy is highly enhanced by a cold rolling. The apparent activation energy of the Al₃Sc particles formation and/or coarsening and that of the Al₆Mn and/or Al₆(Mn,Fe) particle precipitation in the powder and in the compacted alloys were determined. The cold deformation has no effect on the apparent activation energy values of the Al₃Sc-phase and the Al₆Mn-phase precipitation.     

Microstructural evolution of Al–Zn–Mg–Cu alloy during homogenization

In this study, the microstructural evolution of an as-cast Al–Zn–Mg–Cu alloy (AA7085) during various homogenization schemes is investigated. It is found that in a single-stage homogenization scheme, some of the primary eutectic gets transformed into the Al₂CuMg phase at 400 °C, and the primary eutectic and Al₂Cu phase gradually dissolve into the alloy matrix at 450 °C. The Al₃Zr particles are mainly precipitated at the center of the grain because Zr is peritectic. However, the homogeneous distribution of the Al₃Zr particles improves and the fraction of Al₃Zr particles increases in two-stage homogenization scheme. At the first low-temperature (e.g., 400 °C) stage, the Al₃Zr particles are homogeneously precipitated at the center of the grain by homogeneous nucleation and may be heterogeneously nucleated on the residual second-phase particles at the grain boundary regions. At the second elevated-temperature (e.g., 470 °C) stage, the Al₃Zr nuclei become larger. A suitable two-stage homogenization scheme for the present 7085-type Al alloy is 400 °C/12 h + 470 °C/12 h.     

Effect of annealing on the microstructure, room-temperature strength, and fracture toughness of Al2O3−ZrO2−TiN ceramics

The microstructure, phase composition, room-temperature flexural strength, and fracture toughness of Al₂O₃−ZrO₂−TiN (AZT) ceramics were studied on specimens annealed in air at 1000, 1200, and 1400°C. The strength of the ceramics decreased with annealing temperature. The degradation in strength was caused by defects formed on or near the surface of the ceramics during oxidation of TiN which started at 600–700°C. The surface defects after annealing are influenced by the formation of rutile (TiO₂) at 1000 and 1200°C, aluminum titanate (Al₂TiO₅), and titanium suboxide Ti₅O₉ at 1400°C as well as by diffusion processes associated with ZrO₂. If the annealing of smooth AZT specimens in air resulted in lower strength, specimens in the form of single-edge notched beam (SENB) exhibited a considerable increase in fracture toughness (K _Ic) with annealing temperature. Such behavior was caused by the formation of an oxide layer which hindered the propagation of the main crack from the notch base. Thermal treatment of the smooth AZT specimens and further edge notching and testing did not result in a change of K _Ic values. The Al₂O₃ and Al₂O₃−ZrO₂ ceramics were also tested for comparison. Translated from Problemy Prochnosti, No. 1, pp. 132–138, January–February, 1999.     

Electrical and tensile properties of Cu-ThO2, Au-ThO2, Pt-ThO2 and Au-Al2O3, Pt-Al2O3 alloys

Dispersion-strengthened alloys of Pt, Au and Cu containing ThO₂ and Al₂O₃ were prepared by precipitating the elements from a solution containing a suspension of the oxide phase. The precipitate deposited on the oxide particles of 0.05μm average diameter and produced dispersions of good homogeneity on compaction. Alloys containing less than 2 vol% oxide phase had sufficient ductility to permit fabrication of wire. Tensile strength and elongation, hardness, and electrical resistivity were measured as a function of temperature up to 1000°C. The dispersion-strengthening caused a relatively small increase in the resistivity of the alloys compared to the resistivity of the metals. The alloys are useful where high electrical or thermal conductivity combined with superior tensile strength, hardness and oxidation resistance at elevated temperatures, are desirable.     

Properties of Heavily Mn-doped GaMnAs with Curie Temperature of 172.5 K

The authors have investigated the magnetic properties of heavily Mn-doped ferromagnetic semiconductor Ga_1−x Mn _x As thin film with the Mn concentration x of 15.2% grown by molecular-beam epitaxy at relatively high growth temperature of 250 °C. Magnetic circular dichroism and the anomalous Hall effect measurements indicate that this thin film holds the intrinsic ferromagnetic semiconductor features. By low-temperature annealing, the resistivity was significantly decreased and the Curie temperature was largely enhanced from 95 K to 172.5 K.     

Fabrication and magnetoresistivit of ex-situ processed MgB<Subscript>2</Subscript>/Fe monofilament tapes without any intermediate annealing

We have fabricated MgB₂/Fe monofilament wires and tapes by a powder-in tube (PIT) technique, using an ex-situ process without any intermediate annealing. MgB₂/Fe monofilament tapes were annealed at 650–1,050°C for 60 min and 950°C for 30–240 min. We have investigated the effect of annealing temperatures and times on the formation of MgB₂ phase, activation energy, temperature dependence of irreversibility field H _irr(T) and upper critical field H _c2(T), transition temperature (T _c), lattice parameters (a and c), full width at half maximum, crystallinity, resistivity, residual resistivity ratio, active cross-sectional area fraction and critical current densities. We observed that the activation energies of the MgB₂/Fe monofilament samples increased with increasing annealing temperature up to 950°C and with increasing annealing time up to 60 min while it decreased with increasing magnetic field. For the MgB₂/Fe monofilament tape, the slope of the H _c2–T and H _irr–T curves decreased with increasing annealing temperature from 850 to 950°C as well as with increasing annealing time from 30 to 60 min. The transport and microstructure investigations show that T _c, J _c and microstructure properties are remarkably enhanced with increasing annealing temperature. The highest value of critical current density is obtained for the sample annealed at 950°C for 60 min. The J _c and T _c^offset values of the sample annealed at 950°C for 60 min were found to be 260.43 A/cm² at 20 and 38.1 K, respectively.     

Corrosion characteristics of anodized Ti–(10–40wt%)Hf alloys for metallic biomaterials use

The effect of anodizing on corrosion resistance of Ti–xHf alloys has been investigated. Ti–xHf alloys were prepared and anodized at 120, 170 and 220 V in 1 M H₃PO₄ solution, and crystallized at 300 and 500°C. Corrosion experiments were carried out using a potentiostat in 0.15 M NaCl solution at 36.5 ± 1°C. The Ti–xHf alloys exhibited the α′ and anatase phases. The pore size on the anodized surface increases as the applied voltage is increased, whereas the pore size decreases as the Hf content is increased. The anodized Ti–xHf alloys exhibited better corrosion resistance than non-anodized Ti–xHf alloys.     

Dependence of the electrical and optical properties of sputter-deposited ZnO:Ga films on the annealing temperature,time, and atmosphere

Effects of annealing process parameters such as annealing temperature, time, and atmosphere on the electrical resistivity and transmittance properties of Ga-doped ZnO (ZnO:Ga) thin films deposited on glass by rf magnetron sputtering were investigated. The electrical resistivity of a ZnO:Ga thin film is effectively decreased with increasing annealing temperature and time in a reducing atmosphere such as N₂ + 5%H₂. This is attributed to passivation of grain boundaries and zinc ions by hydrogen atoms resulting in increases in carrier concentration and mobility. Also the resistivity of 4.9 × 10⁻⁴Ω cm was obtained by annealing at 200°C for 15 h in the same atmosphere, which is not bad for a transparent conductor for solar cell applications. However, annealing at a temperature higher than 400°C is less effective. The lowest resistivity of 2.3 × 10⁻⁴Ω cm was obtained by annealing at 400°C for 1 h in an N₂ + 5%H₂ atmosphere. The optical transmittance of the ZnO:Ga film is improved by annealing regardless of the annealing atmosphere. Annealing in N₂ + 5%H₂ atmosphere widens the optical band gap, while annealing in an O₂ atmosphere makes the band gap narrower, which can be explained as a blue shift phenomenon.     

Room Temperature Giant Hall Effect in (Ni61Fe39) x (Al2O3)1−x Percolating Nanogranular Films

A series of (Ni₆₁Fe₃₉) _x (Al₂O₃)_1−x films were prepared using the magnetron sputtering technique. The maximum of saturated Hall resistivity 4.06 μΩ⋅cm was observed in (Ni₆₁Fe₃₉)₆₀(Al₂O₃)₄₀ nanogranular film at room temperature, which was about two orders larger than that of pure ferromagnetic metallic films. For the first time, the composition in the atomic fraction at the quantum percolation threshold was accurately characterized by the Rutherford backscattering (RBS) channelling technique in order to substantiate the newly metal-insulator fraction of percolation threshold in the Giant Hall Effect. It also was identified from the TEM image of an as-deposited sample that this large enhancement of the Hall resistivity coefficient was interrelated with the percolation threshold. With a different annealing temperature (T _A ) up to 300 °C , the saturated Hall resistivity of (Ni₆₁Fe₃₉)₆₀(Al₂O₃)₄₀ granular film decreased only a little, which showed its good thermal stability for potential application.     

Metallography and resistivity measurements on a 2–17 type alloy

Metallography and electrical resistivity measurements (ρ _t /ρ _o ) were carried out on an isothermally aged bulk alloy with a substitution composition of Sm(Co_0.67Cu_0.08Fe_0.22Zr_0.028)_8.45. The as-cast alloy was found to consist of four phases: (A) zirconium-rich phase, (B) samarium- and copper-rich phase, (C) cobalt- and iron-rich phase, and (D) very rich in zirconium phase. After annealing at 1170 °C for 5 h, phase B entered into solid solution, suggesting that the other three phases are the stable phases in this system at this temperature. Large decreases in the electrical resistivity were observed after isothermal ageing at temperatures between 650 and 900 °C inclusive. After an initial decrease in the resistivity values at 650, 700, 750 and 800 °C an increase was observed leading to small peaks. The height of this maximum decreased with increasing ageing temperature and disappeared at 830 °C. This effect can be ascribed to the solubility variations, and an activation energy has been derived from the resistivity peaks.     

Synthesis of hexagonal Al2−x Cr x O3 nanodisks by a thermal decomposition of mesoporous Cr4+:Al2O3 powders

Monodispersed hexagonal Al_2−x Cr _x O₃ nanodisks are synthesized through a reactive doping of Cr⁶⁺ cations in a hydrogenated mesoporous AlO(OH)·αH₂O powder followed by annealing at 1,200 °C in air. The reaction was carried out by a drop wise addition of an aqueous Cr⁶⁺ solution (0.5–1.0 M) to AlO(OH)·αH₂O, at room temperature. Al_2−x Cr _x O₃ nanostructure formation was controlled by the nucleation and growth from the intermediate amorphous mesoporous Cr⁴⁺:Al₂O₃ composites in the temperature range 400–1,000 °C. The nanodisks of ∼50 nm diameter and thickness of ∼16 nm is observed in the sample with x of 0.2 and similar nanodisks with a low dimension is observed at a higher value of x of 1.6 (after 2 h of heating at 1,200 °C). The Cr³⁺ ↔ Al³⁺ substitution, x ≤ 1.2, inhibits grain growth in small crystallites. The crystallites in x = 0.2 composition have 43 nm diameter while it is 15 nm in those with x = 1.2 composition.     

Effects of pre-ageing and cold working on grain-interior and grain-boundary reactions of Ag-Pd-Cu alloys

The effects of pre-ageing and cold working on grain-interior and grain-boundary reactions of Ag-Pd-Cu alloys were investigated by electrical resistivity measurements, hardness tests, and optical microscopic observations. Hardness values of the grain interior after the final thermomechanical treatment increased 20%–30% above the values after conventional ageing. The hardness values of alloys preaged at 400°C for 1 min and then cold worked at 30% are the highest (H_v=320).     

X-ray diffraction and magnetic characterization of the retained austenite in a chromium alloyed high carbon steel

In the present work the amount of retained austenite present in quenched and tempered high carbon–chromium alloyed steel was quantified by X-ray diffraction and magnetization saturation measurements. The steel was forged and directly quenched. The retained austenite partially transformed into martensite on cooling down to −196 °C. The M_f temperature of about −150 °C was found by thermomagnetic analysis. Tempering at low temperatures (220 °C and 270 °C) promoted the stabilization effect of austenite. The intrinsic magnetization of the ferromagnetic martensite used in the phase quantification was 206.4 A² m/kg. The increase of the tempering temperature above 320 °C slightly decreases the m _s value of the martensite due to tempering reactions.     

Influence of low-temperature annealing on the properties of Y1Ba2Cu3O7−δ thin films

The influence of annealing at 180 °C on the structure, critical temperature, and electrical resistivity of Y₁Ba₂Cu₃O_7−δ thin films has been investigated. It is shown that films grown at reduced temperatures are sensitive to this annealing, which can substantially alter these film parameters. Pis’ma Zh. Tekh. Fiz. 24, 55–58 (January 12, 1998)     

Nanoscale precipitation and mechanical properties of Al-0.06 at.% Sc alloys microalloyed with Yb or Gd

Dilute Al-0.06 at.% Sc alloys with microalloying additions of 50 at. ppm of ytterbium (Yb) or gadolinium (Gd) are studied with 3D local-electrode atom-probe (LEAP) tomography for different aging times at 300 °C. Peak-aged alloys exhibit Al₃(Sc_1−x Yb _x ) or Al₃(Sc_1−x Gd _x ) precipitates (L1₂ structure) with a higher number density (and therefore higher peak hardness) than a binary Al-0.06 at.% Sc alloy. The Al–Sc–Gd alloy exhibits a higher number density of precipitates with a smaller average radius than the Al–Sc–Yb alloy, leading to a higher hardness. In the Al–Sc–Gd alloy, only a small amount of the Sc is replaced by Gd in the Al₃(Sc_1−x Gd _x ) precipitates, where x = 0.08. By contrast, the hardness incubation time is significantly shorter in the Al–Sc–Yb alloy, due to the formation of Yb-rich Al₃(Yb_1−x Sc _x ) precipitates to which Sc subsequently diffuses, eventually forming Sc-rich Al₃(Sc_1−x Yb _x ) precipitates. For both alloys, the precipitate radii are found to be almost constant to an aging time of 24 h, although the concentration and distribution of the RE elements in the precipitates continues to evolve temporally. Similar to microhardness at ambient temperature, the creep resistance at 300 °C is significantly improved by RE microalloying of the binary Al-0.06 at.% Sc alloy.     

Some aspects on the microstructure and crystallization of rapidly solidified Al-27% Mn alloy

In a previous paper we reported observations of the icosahedral quasistructure (m \(\bar 3 \bar 5\) symmetry) in Al-14 wt % Mn ribbons. In this paper, the microstructure of rapidly solidified Al-27 wt % Mn ribbons is studied where, in addition to the icosahedral phase, the decagonal quasistructure (10/m or 10/m m m symmetry) is also found to occur along with the equilibrium Al₆Mn and Al₄Mn phases, as well as Al. The effect of annealing (in the range 400 to 600° C for 1 to 100 h) on the stability of these structures was studied, using X-ray diffraction and transmission electron microscopy. While the icosahedral phase becomes unstable at 400° C and crystallizes into Al₆Mn, the decagonal phase is seen to persist even after 500° C/100h. The existence of the decagonal phase at 600° C together with the Al₄Mn phase suggests that the decagonal phase arises from a commensurate → incommensurate transformation due to atomic displacement within the Al₄Mn phase.     

Effect of annealing parameters on the magnetic properties of NiZn ferrite thin films

Ni_0.5Zn_0.5Fe_2.0O_4.0 thin films (NZFs) were deposited on Si (100) substrate by a sol–gel method, and the effects of annealing parameters on the structure and magnetic properties of the proposed films were investigated. Moderate heating rate was beneficial to the nucleation of NZFs. When the heating rate was 2 °C/min the saturation magnetization (M _s) achieved its maximum and the coercivity (H _c) reached its minimum. Both the crystallization and M _s of NZFs enhanced with increasing annealing time; however, H _c changed contrarily. High quenching temperature produced a large stress and consequently deteriorated magnetic properties. The optimal annealing parameters of NZFs were annealed at 700 °C, heating rate 2 °C/min, annealing time 1 h, and gradually cooled to room temperature. Finally, NZFs showed a high magnetization of 320 emu/cm³ and low coercivity of 86 Oe.     

Annealing effect on the structural,electrical and 1/f noise properties of Mn–Co–Ni–O thin films

Thin films of Mn_1.4Co_1.0Ni_0.6O₄ (MCN) spinel oxide are grown by radio frequency (RF) magnetron sputtering method on amorphous Al₂O₃ substrate. We investigate the annealing effect on the micro structural and electrical properties of RF sputtered MCN films. It is found that the crystallinity of MCN film is improved with increasing annealing time at 750 °C, and the annealed films present excellent cubic spinel (220) preferred orientation in X-ray diffraction patterns. Comparing to as-sputtered thin film, the annealed films show a decrease of 60 to 70 % in resistivity at 300 K. The annealed samples with post annealing time longer than 18 min acquire a negative temperature coefficient of resistance of about ?3.73 %K^?1 and resistivity of about 210–220 Ω cm at 300 K. 1/f noise of MCN films are also studied and the Hooge’s parameters (γ/n) are calculated. After annealing for 18 to 90 min, the γ/n values of the films are on the order of 10^?21 cm³, which ranks about two orders lower than that of amorphous silicon.     

Grain growth of copper films prepared by chemical vapour deposition

Copper films having thickness 600 nm were prepared on TiN using chemical vapour deposition (CVD). The deposited films were annealed at various temperatures (350–550°C) in Ar and H₂(10%)-Ar ambients. The changes in the grain size of the films upon annealing were investigated. Annealing in an H₂(10%)-Ar ambient produced normal grain growth; annealing in an Ar ambient caused grain growth to stop at 550°C. The grain size followed a monomodal distribution and the mean size increased in proportion to the square root of the annealing time, indicating the curvature of the grain is the main driving force for grain growth. Upon annealing at 450°C for 30 min in an H₂(10%)-Ar ambient, the average grain size of the film increased from 122 nm to 219 nm, and the resistivity decreased from 2.35 μΩ cm to 2.12 μΩ cm at a film thickness of 600 nm. This revised version was published online in July 2006 with corrections to the Cover Date.