J.A. Wilson

Dispersion strengthening in vanadium microalloyed steels processed by simulated thin slab casting and direct charging Part 1 – Processing parameters, mechanical properties and microstructure

Abstract A study simulating thin slab continuous casting followed by direct charging into an equalisation furnace has been undertaken based on six low carbon (0·06 wt-%) vanadium microalloyed steels. Mechanical and impact test data showed that properties were similar or better than those obtained from similar microalloyed conventional thick cast as rolled slabs. The dispersion plus dislocation strengthening was estimated to be in the range 80–250 MPa. A detailed TEM/EELS analysis of the dispersion sized sub 15 nm particles showed that in all the steels, they were essentially nitrides with little crystalline carbon detected. In the steels V–Nb, V–Ti and V–Nb–Ti, mixed transition metal nitrides were present. Modelling of equilibrium precipitates in these steels, based on a modified version of ChemSage, predicted that only vanadium rich nitrides would precipitate in austenite but that the C/N ratio would increase through the two phase field and in ferrite. The experimental analytical data clearly point to the thin slab direct charging process, which has substantially higher cooling rates than conventional casting, nucleating non-equilibrium particles in ferrite which are close to stoichiometric nitrides. These did not coarsen during the final stages of processing, but retained their highly stable average size of, ∼7 nm resulting in substantial dispersion strengthening. The results are considered in conjunction with pertinent published literature.

Evolution of precipitates, in particular cruciform and cuboid particles, during simulated direct charging of thin slab cast vanadium microalloyed steels

Abstract A study has been undertaken of four vanadium based steels which have been processed by a simulated direct charging route with processing parameters typical of thin slab casting, where the cast product has a thickness of 50 to 80 mm (in this study 50 mm) and is fed directly to a furnace to equalise the microstructure prior to rolling. In the direct charging process, cooling rates are faster, equalisation times shorter, and the amount of deformation introduced during rolling less than in conventional practice. Samples in this study were quenched after casting, after equalisation, after the fourth rolling pass, and after coiling, to follow the evolution of microstructure. The mechanical and toughness properties and the microstructural features might be expected to differ from equivalent steels which have undergone conventional processing. The four low carbon steels (~0.06 wt-%) which were studied contained 0.1 wt-%V (V – N), 0.1 wt-%V and 0.010 wt-%Ti (V – Ti), 0.1 wt-%V and 0.03 wt-%Nb (V – Nb), and 0.1 wt-%V, 0.03 wt-%Nb and 0.007 wt-%Ti (V – Nb – Ti). steels V – N and V – Ti contained around 0.02 wt-% N, while the other two contained about 0.01 wt-%N. The as cast steels were heated at three equalising temperatures of 1050°C, 1100°C, or 1200°C and held for 30 – 60 min before rolling. Optical microscopy and analytical electron microscopy, including parallel electron energy loss spectroscopy (PEELS), were used to characterise the precipitates. In the as cast condition, dendrites and plates were found. Cuboid particles were seen at this stage in steel V – Ti, but they appeared only in the other steels after equalisation. In addition, in the final product of all the steels, fine particles were seen, but it was only in the two titanium steels that cruciform precipitates were present. PEELS analysis showed that the dendrites, plates, cuboids, cruciforms, and fine precipitates were essentially nitrides. The two Ti steels had better toughness than the other steels but inferior lower yield stress values. This was thought to be, in part, due to the formation of cruciform precipitates in austenite, thereby removing nitrogen and the microalloying elements, which would have been expected to precipitate in ferrite as dispersion hardening particles.

Improving the analysis of small precipitates in HSLA steels using a plasma cleaner and ELNES

The change from producing high strength low alloy (HSLA) steel sheet by conventional thick slab casting to producing it by direct charged thin slab casting causes a major change in the evolution of the precipitation. A key area of interest is the composition of the sub-10nm precipitates used to produce dispersion hardening. Carbon extraction replicas are frequently used to study precipitates in steels and other metals. When used with annular dark field imaging, this technique gives high contrast images of the precipitates while the thin carbon film adds little background or additional characteristic signals to either electron energy loss spectra or energy dispersive X-ray spectra. The method has the additional major advantage of removing the ferromagnetic matrix when studying HSLA steels. However, when the precipitates contain carbon, the C K-edge is dominated by the contribution from the amorphous carbon film. A plasma cleaner can be used to thin this carbon film to approximately 0.5 nm or less and then the contribution from the carbon in the precipitate can be separated from that in the carbon film using the electron energy loss near edge structure. A similar approach can be taken to separate the oxygen content of the precipitate from that of oxides formed from low-level impurities in the amorphous carbon during the plasma thinning process. In most cases, the precipitate studied here contained little or no oxygen even for the smallest sizes examined (approximately 4 nm). The precipitates contain mainly nitrogen with little carbon. For some compositions, the precipitates are clearly sub-stoichiometric.

A fast beam switch for controlling the intensity in electron energy loss spectrometry

The fast deflection system described in this paper is suitable for controlling the intensity reaching the detector of a magnetic sector electron spectrometer mounted below an analytical transmission electron microscope. Amongst other things, this allows the low loss region of the spectrum to be recorded with the same electron probe conditions used to record core losses, something that is essential for high spatial resolution studies. The plate assembly restricts the width of the electron distribution reaching the viewing screen to a strip approximately 17 mm wide in the direction approximately normal to the dispersion direction of the spectrometer. The resulting deflection has no detectable effect on the FWHM of the zero-loss peak for exposure times as short as 1 micros. At incident energies up to 300 keV, positioning the deflection plates in the 35 mm camera port above the viewing chamber allows voltages of < +/- 3 kV to deflect the electrons out of the spectrometer and beyond the edge of the annular detector. When the deflection is switched on, the electrons are deflected out of the spectrometer in << 40 ns and when the deflection is switched off, the electrons return to within 10 microm of the undeflected position within 100 ns. Thus, even at an exposure time of 30 micros, the smallest time likely to be used in practice with a GATAN 666 spectrometer, < 1% of the signal in the spectrum is from electrons whose scattering conditions differ from those in the undeflected position. The performance of the deflection system is such that it will also be suitable for use with the new and much faster GATAN ENFINA spectrometer system. At incident energies up to 200 keV and possibly up to 300 keV, deflection voltages of +/- 3 kV are sufficient to deflect the electrons off a 1 k x 1 k charge coupled device (CCD) camera placed below the photographic camera. Thus the deflection system can be used as a very fast, non-mechanical shutter for such a CCD camera.

Dispersion strengthening in vanadium microalloyed steels processed by simulated thin slab casting and direct charging Part 2 – Chemical characterisation of dispersion strengthening precipitates

Abstract The compositions of sub-15 nm particles in six related vanadium high strength low alloy steels, made by simulated thin slab direct charged casting, have been determined using electron energy loss spectroscopy (EELS). Such particles are considered to be responsible for dispersion hardening. For the first time, particles down to 4 nm in size have had their composition fully determined. In all the steels, the particles were nitrogen and vanadium rich and possibly slightly substoichiometric carbonitrides. Equilibrium thermodynamics predicted much higher carbon to metal atomic ratios than observed in all cases so that kinetics and mechanical deformation clearly control the precipitation process. Thus it is important to formulate the steel with this in mind.

Gallium oxide and gadolinium gallium oxide insulators on Si δ-doped GaAs/AlGaAs heterostructures

Test devices have been fabricated on two specially grown GaAs/AlGaAs wafers with 10 nm thick gate dielectrics composed of either Ga2O3 or a stack of Ga2O3 and Gd0.25Ga0.15O0.6. The wafers have two GaAs transport channels either side of an AlGaAs barrier containing a Si δ-doping layer. Temperature dependent capacitance-voltage (C-V) and current-voltage (I-V) studies have been performed at temperatures between 10 and 300 K. Bias cooling experiments reveal the presence of DX centers in both wafers. Both wafers show a forward bias gate leakage that is by a single activated channel at higher temperatures and by tunneling at lower temperatures. When Gd0.25Ga0.15O0.6 is included in a stack with 1 nm of Ga2O3 at the interface, the gate leakage is greatly reduced due to the larger band gap of the Gd0.25Ga0.15O0.6 layer. The different band gaps of the two oxides result in a difference in the gate voltage at the onset of leakage of ∼3u2002V. However, the inclusion of Gd0.25Ga0.15O0.6 in the gate insulator introduces man...