High-temperature Localization of Plastic Deformation in Lithium Fluoride Single Crystals

Experimental results on the superlocalization of plastic deformation at high strains and high temperatures in LiF single crystals are described. The physical conditions of transition to a localized plastic flow in the temperature range of 603 K to 1073 K T (0.53–0.94T_mp) using constant strain rate compression tests under strain rates from 10⁻³s⁻¹ to 10⁻²s⁻¹ are found. The results indicate that the deformation mechanism involves dislocation climb, controlled by diffusion. The connection of high temperature flow instability with an excessive concentration of point defects (strain vacancies) in zone of shear has been confirmed.     

Deformation mechanism and dislocation structure of high-purity molybdenum single crystals at low temperatures

High purity molybdenum single crystals were deformed in tension and compression along the symmetric double slip orientation [110] in the temperature range from 300 K down to 0.5 K with strain rates between 10⁻³ and 10⁻⁵ s⁻¹. The activation volume was measured by stress relaxation tests. The dislocation structure of the deformed crystals (T → 1.85 K) was examined by high voltage electron microscopy. It was established that the low temperature increase of the critical shear stress exhibits three distinct temperature regimes with different temperature dependences. These non-uniformities are discussed in terms of recently developed theories of kink-pair formation and kink-kink interactions on screw dislocations in bcc metals. The HVEM observations suggest that the mobility of screw dislocations at very low temperatures should be determined by the combined effects of the PEIERLS barriers and the jog dragging.     

Superplastic flow of a Mg-based bulk metallic glass in the supercooled liquid region

The tensile flow behavior of Mg₆₅Cu₂₅Y₁₀ bulk metallic glass was investigated over a range of strain rates (10⁻³–10⁻¹/s) and deformation temperatures (150–170 °C) in the supercooled liquid region. In this region, the relationship between peak flow stress, strain rate and absolute deformation temperature was described adequately by the classic Sellars–Tegart constitutive relationship. There was also a good correlation between the Zener–Hollomon parameter, Z, and the flow characteristics of the material such as the transition from Newtonian to non-Newtonian flow and maximum achievable tensile elongation; the latter was used for determining the optimum conditions for superplastic flow in the material.     

TEM-Untersuchungen von Gitterfehlern in ZnSiP2-Einkristallen

Results are dealt with concerning TEM investigations of lattice defects in ZnSiP₂ single crystals. After the crystal growth dislocations or stacking faults were found in a few cases only. More frequently twins were present in the microstructure. The crystallographic elements of twinning are {112} 〈111〉. After plastic deformation by bending at 900 °C local dislocation arrangements with high defect density (N_v ≈ 10⁶…︁ 10⁷ cm⁻²) were observed. By means of the diffraction contrast one Burgers vector b = 1/2 〈111〉 could be identified. In some cases the crystals also contained wide deformation stacking faults, which were limited by partial dislocations. The density of twins was not increased under the conditions of deformation reported here. As it can be concluded from investigations of Oettel et al. and from the results of the twin analysis, slip and generation of stacking faults take place on {112}-planes in ZnSiP₂ crystals. Crystallographic considerations on both processes are dealt with.     

Microplasticity of CsI crystals

The study of the mechanisms of plastic deformation of CsI crystals has found the participation of not only the main {110} 〈100〉 slip system but also of the secondary one {110} 〈110〉. Besides that, production and motion of point defects (or small prismatic loops) take place. The gliding on secondary slip system and the deformation accounted for by the generation and motion of point defects is facilitated at low temperatures and high deformation rates. The character of the motion and multiplication of dislocations in the main slip system is investigated. From the temperature and stress dependence of the mobility of isolated dislocations quantitative data on the thermally activated motion of edge dislocations on the main slip system have been obtained. It is shown that, as in the case of other alkali halides, the thermally activated motion of edge dislocations in CsI crystals on {110} 〈100〉 system is limited by their interaction with local obstacles.     

Dislocation internal friction and temperature dependence of yield stress in high-purity molybdenum single crystals

High purity molybdenum single crystals (residual resistivity ratio ≈ 6 · 10⁴) were studied by means of computer-controlled internal friction technique at frequencies of about 100 kHz in the temperature range 6 to 300 K. The amplitude dependences of decrement were measured within the vibrational strain amplitude 10⁻⁷ to 10⁻⁴. It was established that the temperature dependence of ultrasonic amplitude providing a constant level of reversible dislocation deformation coincides well in relative units with the temperature dependence of the critical resolved shear stress at 20 to 180 K.     

Über die röntgenographische Analyse der mittleren quadratischen Atomverschiebungen in einigen Halbleiterkristallen

X-ray measurements of the Debye-Waller factor were performed with single crystals of Ge and of semiconducting compounds A^IIIB^V, A^IIB^VI, A^IVB^VI in the temperature range 100 K — 1000 K. From the results the mean square atomic displacements 〈u²〉 and the Debye characteristic temperatures θ of the materials were calculated. Both parameters are discussed with respect to the influence of the temperature, the influence of point defects and, in the case of the compounds, deviations from the stoichiometric composition on the thermal lattice vibrations. Finally, considerations are presented, concerning the relationship between the parameters 〈u²〉 and θ_M, respectively, and the activation energies of vacancy formation and diffusion in the materials.     

Precision measurements of plastic deformation of β-CuZn at helium temperatures

By attaching condenser plates directly to the tensile specimen, creep rates of β-CuZn single crystals have been measured by the capacitance change in the strain-rate range of 10⁻⁷ to 10⁻⁵ s⁻¹ and at temperatures between 0.7 and 17 K using a ³He cryostat. Slope of the temperature variation of the stress to give a constant strain-rate decreases below 5 K and seems to level off at 0 K. The strain-rate sensitivity becomes almost constant below 2 K. The conventional activation analysis showed that an ARRHENIUS type strain-rate equation breaks down drastically below 5 K. For an effective temperature T^* which gives 2 K at 0 K and asympototically coincides with the testing temperature at 5 K, the experimental results can be fitted to the ARRHENIUS strain-rate equation with an activation enthalpy ΔH(τ) for the PEIERLS mechanism. The above result is interpreted in terms of the quantum-mechanical oscillation of the dislocations.     

Defect structure in nickel single crystals in dependence on the cyclic deformation prehistory

The development of the dislocation structure in nickel single crystals push-pull fatigued at room temperature is investigated for different deformation types using electrical resistivity measurements and results of TEM observations. The dislocation density in the bundles of the matrix is higher after changing the strain amplitude from region A to region B (CD_AB-type) of the cyclic stress-strain curve (N_dB ≈︁ 1.6 ≈︁ 10¹⁵ m⁻²) than after virginal deformation in region B (VD_B-type) especially at higher strain amplitudes (N_dB ≈︁ 0.75 ≈︁ 10¹⁵ m⁻²). Increasing the strain amplitude within region B (CD_BB-type) does not change N_dB. The farther development of the matrix structure after reaching the v_H-minimum during the VD_B-type of deformation suggests the action of the „formation and dissolution”︁ – mechanism, whereas the CD_BB-type causes the „cord”︁-mechanism of the PSB nucleation.     

On the change of low-temperature thermal conductivity of gap after bending

The thermal conduction of a sulphur-doped single crystal plastically deformed by bending at 963 K was measured between 2 and 50 K. The thermal resistivity W at temperatures > 14 K is practically independent on deformation. At lower temperatures W is found to be proportional to AT⁻³ before and to AT⁻³ + BT⁻² after deformation. A is due to boundary scattering, B due to dislocations.     

Electric Characterization of Indium Sesquiselenide Single Crystals

Conductivity, Hall-effect measurements were performed on δ-phase In₂Se₃ single crystals, grown by the Bridgman method over the temperature range 150–428 K, in the directions perpendicular and parallel to the c-axis. The anisotropy of the electrical conductivity and of the Hall coefficient of n-type In₂Se₃ had been investigated. The values of the Hall coefficient and electrical conductivity at room temperature spreads from an order of R_H11 = 1.36 × 10⁴ cm³/coul, σ₁₁ = 4.138 × 10⁻³ Ω⁻¹ cm⁻¹ and R_H = 66.55 × 10⁴ cm³/coul, σ = 0.799 × 10⁻³ Ω⁻¹ cm⁻¹ for parallel and perpendicular to c-axis, respectively. The temperature dependence of Hall mobility and carrier concentration are also studied.     

Dynamic deformation of silicon-rich V3Si single crystals at elevated temperatures

The plastic deformation behaviour of the intermetallic phase V₃Si (Cr₃Si type) was investigated under dynamic conditions. The experiments revealed that V₃Si deforms plastically at a strain rate of about 4.7 × 10⁻⁵s⁻¹ above 1200°. Flow stress depends strongly on deformation temperature and strain rate. An alloy hardening by deviation from stoichiometric composition within the range of homogeneity is observed.     

Plastische Verformung von Siliziumeinkristallen unterschiedlicher Ausgangsversetzungsdichte im Streckgrenzenbereich

Floating-zoned Silicon crystals orientated for single slip both dislocation-free and with grown-in dislocations (EPD₀ = 6,5 · 10⁴ cm⁻²) were dynamically deformed in compression in the temperature range 1120 … 1300 K up to the lower yield point. The dislocation structure of plastically deformed crystals (T = 1138 K; a₀ = 1,45 · 10⁻⁴ s⁻¹) was examined by etching and high-voltage electron microscopy. The crystals exhibit essential differences in deformation behaviour and in the resulting dislocation structure. Typical for the dislocation-free basic material are (i) an inhomogeneous deformation in the range of the upper yield point (ii) a greater portion of sessile lomer dislocations at the lower yield point in relation to the crystal with grown-in dislocations. The measured stresses were related to those values calculated from structure data by employing plasticity theory of diamond-like semiconductors.     

Dislocation arrangements in cyclically deformed polycrystalline molybdenum

The present paper deals with the cyclic stress-strain behaviour of polycrystalline molybdenum at room temperature and the dislocation structures built up within this material during the fatigue process. A cyclic stress-strain curve of molybdenum deformed in a strain-controlled and symmetrical push-pull test is shown. At strain amplitudes e_a < 3 × 10⁻³ arrangements of relatively homogeneously distributed dislocations are observed in the stage of the stabilization of mechanical properties. The characteristics of these dislocation arrangements are similar to those of dislocation structures of unidirectionally deformed molybdenum single crystals. At strain amplitudes e_a > 3 × 10⁻³ dislocation structures are developed with an inhomogeneous dislocation distribution (bundles structures). The dislocation density in the surface layers of fatigued specimens shows larger values than within the material. The cyclic deformation after a change from a small deformation amplitude to a larger one, or vice versa, is connected with characteristic changes of dislocation density.     

Annealing effect on electrical and photoconductive properties of Si implanted GaSe single crystal

GaSe single crystals grown by Bridgman method have been doped by ion implantation technique. The samples were bombarded in the direction parallel to c‐axis by Si ion beam of about 100 keV to doses of 1 × 10¹⁶ ions/cm² at room temperature. The effects of Si implantation with annealing at 500 and 600 °C on the electrical properties have been studied by measuring the temperature dependent conductivity and photoconductivity under different illumination intensities in the temperature range of 100–320 K. It is observed that Si implantation increases the room temperature conductivity 10⁻⁷ to 10⁻³ (Ω‐cm)⁻¹ depending on the post annealing temperature. The analysis of temperature dependent conductivity shows that at high temperature region above 200 K, the transport mechanism is dominated by thermal excitation in the doped and undoped GaSe samples. At lower temperatures, the conduction of carriers is dominated by variable range hopping mechanism in the implanted samples. Annealing of the samples at and above 600 °C weakens the temperature dependence of the conductivity and photoconductivity. This indicates that annealing of the implanted samples activates Si‐atoms and increases structural deformations and stacking faults. The same behavior was observed from photoconductivity measurements. Hence, photocurrent‐illumination intensity dependence in the implanted samples obeys the power low I_pc ∝ Φⁿ with n between 1 and 2 which is an indication of continuous distribution of localized states in the band gap. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Debye–Waller factor approaching the glass-transition temperature in phosphate glasses

The temperature dependence of the mean square displacement, 〈u²〉, calculated by elastic neutron scattering for two phosphate glasses, (AgI)_x(AgPO₃)_1−x with x = 0.3, 0.55, is analysed. The studied samples are probed in a wide range of temperatures going from a few tens of K up to the glass transition temperature and well into the undercooled liquid state. In the low temperature regime a solid like behaviour appears, showing a linear temperature dependence of the Debye–Waller factor, while around T_g the onset of a pronounced increase of 〈u²〉 is observed. The temperature dependence of the normalized elastic intensity and the drawn out Debye–Waller factor are fitted and analyzed by the theoretical previsions of Mode Coupling Theory finding a good agreement.     

EPR-spectrum of irradiated potassium dichromate single crystals

EPR-spectra of X-irradiated potassium dichromate crystals are studied at various temperatures from RT to LNT. The most intensive lines are interpreted as due to radicals CrO₄³⁻ (A-lines) and CrO₃⁻ (C-lines), resulting from Cr₂O₇ owing to X-irradiation. Hyperfine structure of C-line, due to interaction of unpaired electron with Cr⁵³ nucleus, occurs at low temperatures, and new unobserved earlier Q-lines appear near-by C-line. The spectrum may be described by usual spin Hamiltonian for S = 1/2 with following parameters: for A-line gz = 1.9841, gy = 1.9685, gx = 1.9592; for C-line gz = 1.9148, gy = 1.9671, gx = 1.9886, |Az| = 30.53 · 10⁻⁴ cm⁻¹, |Ax| = 10.62 · 10⁻⁴ cm⁻¹, |Ay| = 6.62 · 10⁻⁴ cm⁻¹.     

Dislocation etching in V3Si

Dislocations in as-grown and in plastically deformed V₃Si single crystals have been studied by chemical etching. In as-grown crystals dislocations are partly arranged in small-angle boundaries parallel to {001}, {011}, and {112} planes. The total dislocation density amounted to (10⁵−10⁶) cm⁻². After plastic deformation at elevated temperatures indications for slip and climb processes were observed. The dislocation density increased to 10⁷ cm⁻².     

Crystallizaton Characteristics of the Alternating Tetrafluoroethylene-Ethylene Copolymer

The alternating tetrafluoroethylene-ethylene (TFE-E) copolymer has been studied with respect to its crystallization by using differential scanning calorimetry and optical microscopy. The value of the specific surface energy σ at the melt/crystal interface is calculated to be about 2 · 10⁻³ J/m². The nucleating activity Φ of TiO₂ particles introduced into TFE-E copolymer is estimated to be approximately 0.9. The temperature dependence of the nucleation rate and of the linear growth velocity are constructed in the whole region from the melting temperature T_m to the vitrification temperature T_g. The minimum cooling rate for the formation of a crystal-free TFE-E copolymer glass is calculated and its value amounts to 10⁴ K · min⁻¹.     

X-ray diffraction study of TiN coatings sputtered at different substrate temperatures

Microstructure evolution in TiN films reactively sputtered on steel substrates was investigated by X-ray diffraction. Systematic changes of lattice parameters, texture, internal strain, and macrostress with increasing nitrogen flow into the magnetron deposition chamber were studied for the samples deposited at two different substrate temperatures (150 and 400 °C), and non-monotonic dependences were found for all the quantities. A preferred orientation of the 〈111〉 type for substoichiometric samples is changed to the strong 〈110〉 texture at high nitrogen flow. The largest microhardness was observed for the strongly substoichiometric and very defective films. A marked anisotropy of X-ray line broadening and lattice parameters was found for these samples. The influence of the higher substrate temperature on microstructure of the films is small for all the measured quantities at the deposition rate used (0.06–0.2 μm · min⁻¹).