Crystallographic analysis of nano-structured bainitic steels

A 0.79C-1.5Si-1.98Mn-0.98Cr-0.24Mo-1.06Al-1.58Co (wt%) steel was isothermally heat treated at 200 and 350°C bainitic transformation temperatures. The microstructure was consisted of bainitic ferrite lath and retained austenite for both heat treatment conditions. The crystallographic analysis revealed that the bainitic ferrite laths are close to the Nishiyama-Wassermann orientation relationship with their parent austenite. The isothermal bainite transformation temperature has a significant effect on the retained austenite characteristics and the variant selection of the bainitic ferrite laths. In general, a decrease in the isothennal bainite transformation temperature refined the bainitic structure and weakened the variant selection.

Crystallographic analysis of nanobainitic steels

Electron back-scattered diffraction in conjunction with transmission electron microscopy was employed to investigate the crystallographic nature of bainitic laths formed at relatively low transformation temperatures where a nanostructured bainite forms. It was revealed that the bainitic ferrite laths are close to the Nishiyama–Wasserman orientation relationship with the parent austenite. Furthermore, the temperature showed a significant effect on the retained austenite characteristics and the variant selection of the bainitic ferrite laths. A decrease in temperature generally refined the bainitic structure and weakened the variant selection.

Crystallographic analysis of intervariant boundaries in a lath martensite

In the current study, the crystallographic of intervariant boundary planes distribution in the lath martensite has been measured as a function of lattice misorientation and boundary plane orientation using five macroscopic parameters approach. The distribution revealed a relatively high anisotropy with a tendency for the lath interfaces to terminate on (110) planes. This results from the crystallographic constraints associated with the shear transformation rather than a low energy interface configuration. The lath martensite habit plane was determined to be mostly (110) or near (110). The relative populations of boundaries with [111] and [110] misorientations were greater than other high index misorientations, mostly characterised as (110) symmetric tilt and (110) twist boundary types, respectively.

Efficient formal synthesis of (±)-hyphodermin B

An efficient formal synthesis of hyphodermin B 1, a metabolite of Hyphoderma radula, has been completed in 15% overall yield. The tricyclic carbon skeleton 3 was rapidly assembled from a novel vinyl enone via a Diels−Alder reaction, followed by dehydrogenation and anhydride formation. Selective reduction of anhydride 3 with LiAlH(t-BuO)3 gave hyphodermin B 1 in 99% yield. The structure of hyphodermin B 1 was confirmed by X-ray crystallographic analysis. The anhydride 3, bearing a γ-carbonyl group, displayed unexpected reactivity with the anhydride carbonyl closest to the γ-ketone being the most electrophilic site. This was confirmed by HF/6-31G* calculations. In the presence of base, 3 underwent a rearrangement to the novel lactone 16.

Understanding of the bainite transformation in a nano-structured bainitic steel

A 0.79C-1.5Si-1.98Mn-0.98Cr-0.24Mo-1.06Al-1.58Co (wt%) steel was isothermally heat treated at 200°C for 10 days to form a nano-scale bainitic microstructure consisting of nanobainitic ferrite laths with high dislocation density and retained austenite films. The crystallographic analysis using TEM and EBSD revealed that the bainitic ferrite laths are close to the Nishiyama-Wassermann orientation relationship with the parent austenite. There was only one type of packet identified in a given transformed austenite grain. Each packet consisted of two different blocks having variants with the same habit plane, but different crystallographic orientations. The presence of fine C-rich clusters and Fe-C carbides with a wide range of compositions in bainitic ferrite was revealed by Three-dimensional Atom Probe Tomography (APT). The high carbon content of bainitic ferrite compared to the para-equilibrium level of carbon in ferrite, absence of segregation of carbon to the austenite/bainitic ferrite interface and absence of partitioning of substitutional elements between the retained austenite and bainitic ferrite were also found using APT.

Characterization of nano-structured bainitic steel

A 0.79C-1.5Si-1.98Mn-0.98Cr-0.24Mo-1.06Al-1.58Co (wt%) steel was isothermally heat treated at 200°C for 10 days to produce a nano-structured bainitic steel. The microstructure consisted of nanobainitic ferrite laths with a high dislocation density and retained austenite films having extensive twins. The crystallographic analysis using TEM and EBSD revealed that the bainitic ferrite laths are close to the Nishiyama-Wassermann orientation relationship with their parent austenite. There was only one type of packet identified in a given transformed austenite grain. Each packet consisted of two different blocks having variants with the same habit plane, but different crystallographic orientations. Atom Probe Tomography (APT) revealed that the carbon content of nanobainitic ferrite laths was much higher than expected from the para-equilibrium level. This was explained due to the long heat treatment time, which led to the formation of fine Fe-C clusters on areas with high dislocation densities in bainitic ferrite laths.

Recent progress in the development and use of organic ionic plastic crystal electrolytes

Significant progress has been made recently in the development of Organic Ionic Plastic Crystals (OIPCs), a unique family of solid state electrolytes with applications in electrochemical devices such as lithium batteries and dye-sensitised solar cells. The negligible volatility of OIPCs renders them more suitable than molecular species for long-term device use, while the high thermal and electrochemical stability of many OIPCs fulfils an essential requirement for solid state electrolytes for many device applications. However, the complex mechanisms of conduction through these materials, both in their pure state and in the presence of a small amount of a second component (such as lithium salts to enable their use in lithium batteries) are still not fully understood. At the same time, the range of anions and cations utilised in the synthesis of plastic crystal phases continues to increase. This perspective concentrates on recent research into both fundamental and device-oriented aspects of these materials. Important fundamental understanding of the physical properties and transport mechanisms of different OIPCs has been achieved through use of techniques including variable temperature solid-state NMR and crystallographic analysis, as well as detailed molecular dynamics simulations. In parallel, the applicability of these materials as electrolytes for dye-sensitised solar cells and lithium batteries is being more widely demonstrated. The possibility of using OIPCs as solid state electrolytes for fuel cells is also discussed.

Hydrolysis of bis((trimethylsilyl)methyl)tin dihalides. Crystallographic and spectroscopic study of the hydrolysis pathway

The synthesis and characterization by multinuclear NMR spectroscopy of the diorganotin dihalides (Me₃SiCH₂)₂SnX₂ (1, X = Cl; 2, X = Br), the diorganotin dichloride water adduct (Me₃SiCH₂)₂SnCl₂·H₂O (1a), the dimeric tetraorganodistannoxanes [(Me₃SiCH₂)₂(X)SnOSn(Y)(CH₂SiMe₃)₂]₂ (3, X = Y = Cl; 4, X = Br, Y = OH; 5, X = Br, Y = F; 6, X = Y = OH; 8, X = Cl, Y = OH), and the molecular diorganotin oxide cyclo-[(Me₃SiCH₂)₂SnO]₃ (7) are reported. The structures in the solid state of compounds 1a, 3, 6, and 7 were determined by single-crystal X-ray analysis. In toluene solution, the hydroxy-substituted tetraorganodistannoxane 6 is in equilibrium with the diorganotin oxide 7 and water. The eight-membered diorganotin oxide cyclo-[(Me₃SiCH₂)₂SnO]₄ (7a) is proposed to be involved in this equilibrium. On the basis of the results of this and previous works, a general hydrolysis pathway is developed for diorganotin dichlorides containing reasonably bulky substituents.

Electron backscattering diffraction analysis of an ancient wootz steel blade from central India

The electron backscattering diffraction technique was used to analyse the nature of carbides present in an ancient wootz steel blade. Bulky carbides, pro-eutectoid carbide along the prior austenite grain boundaries and fine spheroidized carbides were detected. Electron backscattering diffraction was employed to understand the texture of these carbides. The orientations of the cementite frequently occur in clusters, which points to a common origin of the members of the cluster. For the bands of coarse cementite, the origin is probably large coarse particles formed during the original cooling of the wootz cake. Pearlite formed earlier in the forging process has led to groups of similarly oriented fine cementite particles. The crystallographic texture of the cementite is sharp whereas that of the ferrite is weak. The sharp cementite textures point to the longevity of the coarse cementite throughout the repeated forging steps and to the influence of existing textured cementite on the nucleation of new cementite during cooling.

Conductivity, NMR and crystallographic study of N,N,N,N-tetramethylammonium dicyanamide plastic crystal phases : an archetypal ambient temperature plastic electrolyte material

N,N,N,N-Tetramethylammonium dicyanamide (Me₄NDCA) has been examined via differential scanning calorimetry (DSC), thermogravimetric analysis, conductivity, single crystal X-ray diffraction and ¹H nuclear magnetic resonance (NMR) analyses, and was found to be highly conductive in the solid state (σ =10−3 S cm⁻² at 420 K) and to also exhibit unusual plastic crystal behaviour. To investigate the correlation between such behaviour and the occurrence of molecular rotations in the crystal, ¹H NMR second moment measurements are compared with calculated values predicted from the crystal structure. While DSC analysis indicates a number of solid–solid transitions at ambient temperatures, subsequent ¹H NMR analysis of the Me₄N⁺ cation shows that a variety of rotational motions become active at low (<240 K) temperatures, and that such transitions in rotational states occur over a range of temperatures rather than in a sharp transition. Conductivity analysis reveals that between 320 K and 420 K the conductivity increases by more than six orders of magnitude in the solid state, in line with the transition of the Me₄N⁺ cation to a diffusive state, and that other phase transitions observed in this temperature range have no marked effect on the conductivity. Conduction in this solid state is therefore envisaged to involve a vacancy-diffusion model, involving Me₄N⁺ cation vacancies.

Crystallographic features during martensitic transformation in Ni-Mn-Ga ferromagnetic shape memory alloys

The martensitic transformation crystallography in two Ni ₅₃Mn₂₅Ga₂₂ (at. %) ferromagnetic shape memory alloys (FSMAs) was investigated by means of misorientation calculation and pole figure analysis based on the orientation of the martensitic lamellae obtained from electron backscattered diffraction (EBSD) measurements. In the alloy that was first annealed at 1073K for 4h, and then cooled to 473K at ~4K/min and held for 30min, followed by cooling to room temperature at ~10K/min, there are only two kinds of differently orientated martensitic lamellae with a misorientation angle of ~82° distributed alternatively in each initial austenite grain. There is a compound twinning orientation relationship between the two lamellae. The prevalent orientation relationship between austenite and martensite is Kurdjumov-Sachs (K-S) relationship with (111)_A//(10I)_M, [1-10]_a//[11-1]_m. In the alloy that was annealed at 1173K for 4h followed by furnace cooling, nanoscale twins inside the martensitic lamellae were observed and the orientation relationships both between the nanotwins within one lamella and between the nanotwins in two neighboring lamellae were determined. The results presented in this paper will enrich the crystallographic data of the FSMAs and offer useful information for the development of novel FSMAs with optimal performances.

Variant selection and intervariant crystallographic planes distribution in martensite in a Ti-6Al-4V alloy

The transformation texture was studied in a Ti-6Al-4V alloy for two microstructures produced through different phase transformation mechanisms (i.e. diffusional vs. displacive). Both microstructures revealed qualitatively similar crystallographic texture characteristics, having two main texture components with Euler angles of (90°, 90°, 0°) and (90°, 30°, 0°). However, the overall α texture strength was considerably weaker in the martensitic structure (i.e. displacive mechanism) compared with the α + β microstructure produced through slow cooling (i.e. diffusional mechanism). The intervariant boundary distribution in martensite mostly revealed five misorientations associated with the Burgers orientation relationship. The five-parameter boundary analysis also showed a very strong interface plane orientation texture, with interfaces terminated mostly on the prismatic planes {hki0}, when misorientation was ignored. The highest intervariant boundary populations belonged to the 63.26°/[10 553 ] and 60°/[112 0] misorientations, with length fractions of 0.38 and 0.3, respectively. The former was terminated on (41 3 0), and the latter was a symmetric tilt boundary, terminated on (1 011). The intervariant plane distribution in martensite was determined more by the constraints of the phase transformation than by the relative interface energies.