On the Influence of Short R.T. preageing on the formation of the η′-phase in an Al-Zn(4.5 at.%)-Mg(2.5 at.%) alloy

The influence of short R.T. preageing (1 min) after quenching from 480 °C into RT-water on the formation of the η′-phase in an Al-Zn(4.5)-Mg(2.5) alloys has been investigated by means of TEM, XSAS, resistivity, and hardness measurements in the ageing temperature range between T_a = 120 °C comparing samples directly quenched (DQ) to T_a and those quenched into RT-water, kept there for 1 min, and subsequently stored in an oil-bath of T_a (IQ). At T_a ≦ 170 °C both heat treatments result in finely distributed precipitates of the η′-phase accompanied by a fairly high hardness value. But at T_a ≧ 180 °C the DQ leads only to few coarse heterogeneously formed η′- and η-precipitates, whilst the IQ yields qualitatively the same precipitation structure as already described at T_a ≦ 170 °C even till 280 °C. These results are interpreted assuming that. A1) the limitation temperature of homogeneous formation of η′ is located at about T_h = 175°c and A2) during the pre-ageing at RT “nucleation sites” are formed as already suggested by RYUM, which are able to act as sites for heterogeneous formation of η′ even at T_a > T_h. Hints are obtained that the formation of these “nucleation sites” is not so strongly governed by the quenched-in excess vacancies as discussed in the literature.     

Information on the early decomposition behaviour in Al-Zn(6)-Mg(X) alloys by an analytical description of isothermal resistivity curves

Based on a theoretically derived expression for the extra-resistivity resulting from the formation of GP-Zones isothermal resistivity measurements with Al-Zn(6 at.%)–Mg(0.81; 1.73 at.%) alloys were analysed. A comparison of both expressions d(ln _ϱex)/dt and d(ln f)/dt yields statements on the early stage of decomposition behaviour, especially, whether up to a considered time point size growth happened. The evaluated examples lead to the conclusion that size growth is most probably to exclude up to the time point of 4T. The T_a-dependence of the maximum value of extra-resistivity is explained by an equilibrium distribution of bigger particles of a smaller number at higher aging temperatures, of smaller particles of a greater number at lower aging temperatures and by the assumption, that the amount of solute atoms inside the GP-zones is decreasing with rise of T_a.     

On the influence of the pre-ageing temperature on the reversion behaviour of an Al-4.5 at.% Zn-2.0 at.% Mg alloy

The reversion behaviour of an Al-Zn(4.5)-Mg(2.0) alloy was investigated by SAXS in dependence of the pre-ageing temperature, T_pre, (ranging between 60°C and 100°C) and the reversion temperature, T_rev, (120°C till 200°C) starting with precipitates having a radius of (1.2 ± 0.1) nm and (1.5 ± 0.1) nm, respectively. During the reversion treatment applied up to T_rev = 160°C three stages could be distinctly distinguished, namely the dissolution of unstable zones, the growth of the stable zones on the expense of the dissolved one, and at last the coarsening of the precipitates by the OSTWALD-ripening process, where the structure changes become independent of the pre-history (start radius). The change of T_pre from 60°C to 100°C does not influence the structure changes going on at T_rev, that means between 60°C and 100°C the same type of G.P. zones grows.     

On the structure of α′m-precipitates in Al-Zn alloys

The lattice parameter of the f.c.c. α′-phase in an Al-12at.% Zn alloy decomposed at ageing temperatures ranging between 170 °C and 210 °C was investigated by an analysis of Moiré fringe contrasts which appear inside the precipitates in the TEM-micrographs. Additionally information was gained concerning the relationship between the corresponding lattice of the α′_m-precipitates and the matrix. The analysis proved that the misfit between the lattice of the α′_m-precipitates and the adjoining matrix is fairly small, namely less than 1.5% in lattice spacing and less than 1° in the angular rotation. From these results it was concluded that the major part of the matrix planes passes the precipitates without interruption.     

Structural Changes during Post-Ageing of an Al-Zn (15 at.%) Alloy between 125 °C and 215 °C

The structural changes going on in an Al Zn (15 at.%) alloy postaged between 125 °C and 215 °C after pre-ageing between 20 °C and 90 °C (till start r_s = (20…︁ 55) Å are obtained) were followed by means of XSAS-investigations. The main results are the following:

• 1 An increase of r_s does not favour the growth of the precipitates during the reversion treatment.
• 2 At later reversion times the happening is obviously independent of the pre-history of the samples.
• 3 The integral intensity is decreasing with increase of T_rev, but the mean distance (d)-size (r_G) relation between the precipitates is not changed remarkably up to T_rev ≈ 200 °C in the early reversion stage.

Conclusions from this behaviour are drawn.     

Determination of the phase ranges during cooling and heating of Al-40wt.%—(0—3) wt.% Mg alloys

The various phases and the respective ranges of their existence were determined during continuous cooling from temperatures close below the solidus line to R.T. with a rate of 2 K min⁻¹ as well as during the subsequent heating in few Al Zn(40 wt.%)–Mg(X) alloys (X = 0; 0.5; 1.0; and 3.0 wt.%) by means of X-ray phase-analysis, small angle X-ray scattering, differential thermo-analysis, optical microscopy, and X-ray micro-analysis. The most striking features are that even addition of only 0.5 wt.% Mg cause the formation of precursors of the MgZn₂ equilibrium phase few degrees below the solidus line.     

The influence of the direct quench and indirect quench to Ta > Th on the decomposition behaviour of an Al-2 at.% Zn-1 at.% Mg alloy

The decomposition behaviour of an Al-2.0 at.% Zn-1.0 at.% Mg alloy after direct quench (DQ) and indirect quench (IQ:T = 23 °C, t) to the ageing temperature T = 160 °C (above the temperature of the rapid homogeneous nucleation, T_h) was investigated by means of TEM and isothermal resistivity measurements. The precipitation density of the η-particles yields a maximum value at pre-ageing times about 10 min at T = 23 °C. To clear up the reason for that phenomenon a loop-formation and clustering model was introduced.     

On the Size Distribution of Guinier-Preston Zones Grown in an Al-4.5 at.% Zn Alloy at Room Temperature

The size distribution SD of the Guinier-Preston (GP) zones grown in an Al-4.5 at.% Zn alloy were determined by analysis of the intensities of the small-angle X-ray scattering (SAXS) curves. Four different methods frequently used in the literature were applied and the obtained results were compared. In addition the SD's obtained by the SAXS methods were compared with that found by high-resolution electron microscopic investigations. – From these comparisons conclusions were drawn.     

On temperature dependence of Debye-Waller factor in V3Si in the temperature range from 8 to 293 K

The temperature dependence of the Debye-Waller factors of vanadium and silicon in V₃Si and that of the X-ray Debye temperature are obtained from the integral intensities of X-ray reflection measured at 11 temperatures ranging from 8 K to 293 K. It shown that the breaks on these curves are observed at T_br = 21.7 K. This fact allows to assume that the phase transition in this compound is accompanied by the rapid change of the atomic vibration frequencies.     

On the reversion behaviour of an Al-15 at.% Zn alloy between 155°C and 175°C

The structural changes going on in an Al-15 at.% Zn alloy postaged in the vicinity of the kink of the C-curve (161°C) in the T.T.T.-diagram after pre-ageing at R. T. or 90°C (till start radii r_S between 1.0 and 4.0 nm were obtained) were followed by means of SAXS-investigations. The main results are the following:

• 1 No indication could be found that the reversion behaviour is remarkably changed by crossing the temperature of the kink of the C-curve in the T.T.T.-diagram, i.e. the reversion as well as the growth mechanism of the zones does not differ considerably below and above 161°C.
• 2 The decrease of the integral intensity Q₀ during the reversion process is mainly due to both the loss of zinc content of the zones and its rise in the matrix and not essentially by the diminution of the volume fraction of the precipitates.
• 3 Zones of a start radius of about 4 nm are much more stable against the decrease of the zine content during the reversion treatment that those of 2 nm.

     

Investigation of the microhardness and the electrical resistivity of undercooled Ni-10 at.% Si alloys

Ni-10 at.% Si alloys (Ni and Si of purity of 99.99%) were prepared by arc melting method under argon atmosphere in a water-cooled copper hearth with a non-consumable tungsten electrode and titanium getter. Spherical-shaped Ni-10 at.% Si alloy melts are undercooled in a containerless electromagnetic levitation apparatus. The effects of undercooling (ΔT) on the microstructure, electrical resistivity (ρ) and microhardness (HV) were investigated. The experimental results reveal that with the increase of the undercooling of the melts from 16 to 110 K, the microstructures undergo transition from coarse dendritic morphology to ultra fine dendritic morphology. The measurements of microhardness of the samples were performed by using a microhardness test device. The dependence of microhardness on undercooling was analyzed and it has been found that with increasing the undercooling the HV increases. Variations of electrical resistivity of the Ni-10 at.% Si alloy with the temperature in the range of 300-800 K were also determined by using a standard d.c. four-point probe technique. The resistivity of samples increases with increasing temperature and undercooling.     

Development of the microhardness of an al-2.0 at.% zn-1.3 at.% mg alloy with additions of technical impurities during a two-step ageing treatment (ii)

The alloy was preaged in the temperature range between T_pre = 50 °C and 160 °C for various times and afterwards postaged at R.T. The course of the microhardness and the related structure changes (TEM and SAXS investigations) were investigated. The main results are the following: – Preageing the samples times less than the incubation time no essential structure changes take place at least not in the sense that the further decomposition happening during the postageing at R.T. is remarkably influenced. – The samples preaged at T_a 110 °C for times somewhat longer than the incubation time show a distinct minimum after the end of the postageing period of 42 d at R.T. Most probably at T_a 110 °C in the starting period of the decomposition nuclei of the α-phase or of spherical hexagonal zones were formed. These nuclei lessen considerably the amount of G.P. zones able to be nucleated during the R.T. postageing.     

On the ordering of Cr1-xAlx alloys (x < 0.33) leading to microprecipitations of X- and β-phases

The analysis of electron diffraction patterns of Cr_1-xAl_x alloys with 0.16 ≦ x ≦ 0.24 has been performed. The diffraction vectors describing the position of X-phase spots were corrected to the new 0.769 < 0.004 〈111〉value. The ordering model of Cr_1-xAl_x alloys with x < 0.33 is discussed in connection with physical properties. The new identification of the X-phase as Cr₄Al displacive modulation structure is proposed.     

An effective growth method to improve the homogeneity of relaxor ferroelectric single crystal Pb(In1/2Nb1/2)O3‐ Pb(Mg1/3Nb2/3)O3‐PbTiO3

Compositional segregation usually has negative effects on the growth of solid solution ferroelectric single crystals of Pb(In_1/2Nb_1/2)O₃‐Pb(Mg_1/3Nb_2/3)O₃‐PbTiO₃ (abbr. PIN‐PMN‐PT or PIMNT). A modified Bridgman method was adopted in this work to control the segregation and improve the compositional homogeneity significantly. The characteristic of this work is to use multiround growths and gradient composition raw materials in order to keep the PbTiO₃ concentration constant during the crystal growth. As an example, the two‐round growth of ternary PIN‐PMN‐PT single crystal is conducted in the same Pt crucible with gradient raw materials, where the first‐round boule was used as the seed crystal for the second‐round growth. Our results show that the as‐grown (Ф80 mm × 270 mm) PIN‐PMN‐PT crystals exhibit higher phase transition temperatures (T_c∼180 °C, T_r/t∼110 °C) and larger coercive field (E_c∼5–5.5 kV/cm), which are much better than the performances of Pb(Mg_1/3Nb_2/3)O₃‐PbTiO₃ crystals, and similar dielectric and piezoelectric performances (ε∼5000, tanδ∼1.25%, d₃₃∼1500 pC/N, k_t∼60%). And about 85 percent of the crystal boule grown by the two‐round growth technique could maintain its compositions around the morphotropic phase boundary.     

Growth of single crystals of cinnabar (α-HgS) at rather low temperature

Synthetic crystals of cinnabar have been grown in a special oven. We have obtained specimens about 3 × 3 × 4 mm³ in size and of average crystalline quality.     

On chemical kinetics of silicon deposition from silane (III). LPCVD poly silicon formation in the temperature range 900–950 K

LPCVD poly Silicon deposition form silane has been investigated for limited conditions regarding temperature, silane input and pumping speed. It has been found that layer growth is controlled by a chemical reaction of 0.5^th-order in consequence of which growth rate linearly decays along the axis of an open isothermal reactor tube. The slope of that decay is determined not only by the reaction rate constant but also by linear gas velocity within the tube and that part of total substrate surface area that is effectively exposed to silane at each wafer position. In conseqence growth rate decay is the steeper not only the higher temperature will be chosen but also the slower gas velocity is adjusted and the smaller wafers are separated to each other. The kind of how axial layer growth rate distribution is effected by changing wafer spacing is a proof for the heterogeneous reaction mechanism. The silicon forming reaction is characterised by an activation energy of about 52 kcal/mole.     

On the temperature dependence of the enthalpies of mixing in liquid binary (Ag, Cu, Ni)-Sn alloys

The partial and integral enthalpies of mixing of liquid binary alloys in the systems Ag-Sn, Cu-Sn and Ni-Sn were determined at different temperatures from 500 to 1500 °C using drop calorimetry techniques. Generally, our measured values fit well to most of the hitherto reported results. The data were fitted using a Redlich-Kister polynomial and the binary interaction parameters were evaluated. For all three systems the enthalpy curves at various temperatures are discussed focusing on the association theory. C^ass,C^A₁,B₁,C^A₁,A_iB_j,C^B₁,A_iB_j, the interaction parameters and K_AiBj were determined. The general shape and supposed temperature dependence of the enthalpy of mixing in Ag-Sn and Cu-Sn could be confirmed. No significant temperature dependence could be found experimentally for Ni-Sn at temperatures above 1100 °C. Extrapolations into the metastable liquid regions based on the association theory, however, indicate a small drop of Δ_MixH with temperature. A second series of measurements limited to low concentrations of Ag, Cu, or Ni, respectively in Sn has been performed in order to determine the partial enthalpies of mixing at infinite dilution at 500, 600, 700, and 800 °C. Temperature dependence could be observed for all three binary systems, most developed for Ni-Sn.     

On the influence of impurity additions and quenching temperature on the course of the microhardness (HV) during a two-step ageing treatment of an Al-2.0 at.%Zn-1.3 at.%Mg Alloy

A pure as well as the analogous technical alloy were directly quenched from T_q = 400 °C or 490 °C to T_a, preaged at T_a (ranging between 50 °C and 160 °C) various times (t_a), and subsequently postaged at R.T. up to t_post = 42 d. — Ageing the samples below the upper limit temperature of the homogeneous formation of G.P. zones (T_hn) no essential difference in the course of the HV-number attained after one- as well as two-step ageing in dependence on the addition of impurity atoms and T_q could be found. — Contrary to this behaviour after pre-ageing at T_a > T_hn and postageing at R.T. a variation of both T_q and the content of impurity atoms shows a considerable effect. The reason is the difference in the density of nucleation sites for heterogeneous formation of precipitates of the η′- and/or η-phase in dependence of T_q and impurity content.