Study of autoabsorption for total α and β counting

The RaMsEs Group (Radioprotection et Mesures Environnementales) of the IPHC performs research and offers services mainly in the field of radioactivity measurements and sample analysis. This report will describe some of our recent experience using a semiautomatic evaporation system to prepare large area thin deposits for total α and β counting and gives experimental and simulated results for the autoabsorption coefficients.     

The Dislocation Structure of a Single-Crystal γ + γ′ Two-Phase Alloy After Tensile Deformation

The dislocation structures of an industrial single-crystal γ + γ′ two-phase alloy DD3 after tensile deformation from room temperature to 1273K were studied by transmission electron microscopy. The strength of this alloy decreased with an increase in the temperature, and showed a strength peak at 1033K. At room temperature, the dislocations shearing the γ′ particles were found to be 1/3<112> partial dislocations on the dodecahedral slip system <112>{111}. Some dislocation pairs on the cubic <110>{100} system that blocked the glide of dislocations were found at a medium temperature of 873K. As a result, dislocation bands were formed. Shearing of γ′ particles by 1/3<112> partial dislocations on the dodecahedral slip system <112>{111} was also found at this temperature. At the peak temperature of 1033K, because of the strong interaction between dislocations on the {111} and {100} planes, the extent of dislocation bands with high dislocation densities was extensive. The 1/3<112> partial dislocations on the dodecahedral slip system <112>{111} also existed. When the temperature reached the high temperature of 1133K, the range of dislocation bands was limited. The γ′ particles were sheared by <110> dislocation pairs on the octagonal <110>{111} system and the cubic <110>{100} system. At 1273K, the regular hexagonal dislocation networks were formed in the γ matrix and at the γ/γ′ interface. The Burgers vectors of the network were found to be b₁ = 1/2[110], b₂ = 1/2[1–10], b₃ = [100], and the last one was formed by the reaction of b₁ + b₂ → b₃. Dislocations shearing the γ′ particles were found to be <110> dislocation pairs on the octagonal system <110>{111} and cubic slip system <110>{100} at 1273K.     

A detector for filtering γ-ray spectra from weak fusion–evaporation reactions out of strong background and for Doppler correction: The recoil filter detector, RFD

A detector has been designed and built to assist in-beam γ-ray spectroscopy with fusion–evaporation reactions. It measures with high efficiency the evaporation residues that recoil out of a thin target into the angular interval from 1.8° to 9.0° at an adjustable distance of 1000–1350 mm from a target, in coincidence with γ-rays detected in a Ge-detector array. This permits filtering of such γ-rays out of a much stronger background of other reaction products and scattered beam. Evaporation residues are identified by their time-of-flight and the pulse height using a pulsed beam. The velocity vector of the γ-emitting recoil is also measured in the event-by-event mode, facilitating to correct the registered γ-ray energy for the Doppler shift, with the resulting significant improvement of the energy resolution. The heavy-ion detection scheme uses emission of secondary electrons caused by the recoiling ions when hitting a thin foil. These electrons are then electrostatically accelerated and focused onto a small scintillator that measures the summed electron energy, which is proportional to the number of electrons. The detector is able to operate at high frequency of the order of 1 MHz and detect very heavy nuclei with as low kinetic energy as 5 MeV. The paper describes the properties of the detector and gives examples of measurements with the OSIRIS, GAREL+ and EUROBALL IV γ-ray spectrometers. The usefulness of the technique for spectroscopic investigations of nuclei with a continuous beam is also discussed.     

Oxidation protective coatings for γ‐TiAl – recent trends

Engine designers show continued interest in γ‐TiAl based titanium aluminides as light–weight structural materials to be used at moderately elevated temperatures. Although alloy development has made significant progress in terms of mechanical properties and environmental resistance, protective coatings have been developed that help to extend the lifetime of these alloys significantly. The major challenge of coating development is to prevent the formation of fast growing titania. Furthermore, changes of coating chemistries at high temperatures have to be considered in order to avoid rapid degradation of the coatings due to interdiffusion between substrate and coating. The paper describes recent work of the authors on different coatings produced by means of magnetron sputter technique. Thin ceramic Ti‐Al‐Cr‐Y‐N layers tested at 900 °C exhibited poor oxidation resistance. In contrast, intermetallic Ti‐Al‐Cr, Si‐based and aluminum rich Ti‐Al coatings were tested at exposure temperatures up to 950 °C for 1000h resulting in reasonable and partially excellent oxidation behaviour.     

Effects of Thermally Induced Cyclic γ ↔ ε Transformation on Shape Memory Effect of a Quenched FeMnSiCrNi Alloy

The effects of thermally induced cyclic γ ? ε transformation on microstructures and shape memory effect (SME) are investigated in a quenched Fe14Mn5.5Si8.0Cr5.0Ni alloy. The results show that the annealing at 773 K remarkably improves the SME in the quenched alloy. One thermal cycling between 290 and 773 K remarkably increases the SME, but the further thermal cycling hardly improves the SME. The reason is that the amount of thermal ε martensite remarkably reduces after annealing at 773 K, but it hardly changes with the further increase of thermal cycling between 290 and 773 K. The pre‐existing thermal ε martensite not only prevents the occurrence of stress‐induced ε martensitic transformation but also promotes the formation of α′ martensite.     

Evidence for η6 Coordination to a Fullerene

Evidence for the first η⁶ derivative of a fullerene, [MoC₆₀F₁₈(CO)₃] has been obtained from reaction between [Mo(CH₃CN)₃(CO)₃] and C₆₀F₁₈.     

Amyloid Self‐Assembly of hIAPP8‐20 via the Accumulation of Helical Oligomers, α‐Helix to β‐Sheet Transition,and Formation of β‐Barrel Intermediates

The self‐assembly of human islet amyloid polypeptide (hIAPP) into β‐sheet‐rich nanofibrils is associated with the pathogeny of type 2 diabetes. Soluble hIAPP is intrinsically disordered with N‐terminal residues 8–17 as α‐helices. To understand the contribution of the N‐terminal helix to the aggregation of full‐length hIAPP, here the oligomerization dynamics of the hIAPP fragment 8–20 (hIAPP8‐20) are investigated with combined computational and experimental approaches. hIAPP8‐20 forms cross‐β nanofibrils in silico from isolated helical monomers via the helical oligomers and α‐helices to β‐sheets transition, as confirmed by transmission electron microscopy, atomic force microscopy, circular dichroism spectroscopy, Fourier transform infrared spectroscopy, and reversed‐phase high performance liquid chromatography. The computational results also suggest that the critical nucleus of aggregation corresponds to hexamers, consistent with a recent mass‐spectroscopy study of hIAPP8‐20 aggregation. hIAPP8‐20 oligomers smaller than hexamers are helical and unstable, while the α‐to‐β transition starts from the hexamers. Converted β‐sheet‐rich oligomers first form β‐barrel structures as intermediates before aggregating into cross‐β nanofibrils. This study uncovers a complete picture of hIAPP8‐20 peptide oligomerization, aggregation nucleation via conformational conversion, formation of β‐barrel intermediates, and assembly of cross‐β protofibrils, thereby shedding light on the aggregation of full‐length hIAPP, a hallmark of pancreatic beta‐cell degeneration.     

Enhanced Grain Refinement Through Deformation Induced α Precipitation in Hot Working of α + β Titanium Alloy

This study reports a novel forging process to fabricate bulk fine‐grained (grain size ≈ 1 µm) Ti–6Al–4V alloy, in which temperatures near the β transus (T_β) and strain rates around 0.15 s^?1 are used for the deformation. The formation of fine‐grained microstructure is mainly result from the deformation‐induced precipitation of α grains from the β matrix.     

Calculation of efficiency functions in 4π β-γ counting

An attempt is made to calculate an efficiency function applicable to 4πβ-γ coincidence measurements as the first stage of evaluating the order of the polynomial of the fitting function. For this purpose, the β-ray energy spectra and self-absorptions of spherical particle sources are calculated by the Monte Carlo simulation under the continuous slowing down approximation. On the other hand, it is shown that three sets of absorption coefficients and partial intensity ratios corresponding to a β-ray group give analytically the self-absorption for the same particle sources. Finally, we show that the efficiency functions applicable to ⁵⁹Fe and ¹³⁴Cs are easily obtained by using the energy spectra or self-absorptions.     

Machining of γ-TiAl

Knowledge of the machining parameters for titanium aluminides of the type γ-TiAl is essential for the acceptance and application of this new heat-resistant light-weight material for high performance components in automobile and aircraft engines. This work evaluates drilling, turning, sawing, milling, electroerosion, grinding, and high-pressure water-jetting of primary castings. The results indicate that there is a potential for each machining process, but a high quality of surface finish can only be achieved by some of the processes.     

Improving long term oxidation protection for γ‐TiAl substrates

In previous work, a thermal spray multilayer system consisting of Zirconia (ZrO₂) and MCrAlY top coat showed promising results regarding the oxidation behavior of the Gamma Titanium Aluminides substrates tested, which encouraged further research activities. Diffusion of substrate material was successfully inhibited by a ceramic Zirconia coating. A building up of a dense and stable oxide layer could be achieved by additional application of an MCrAlY top coat, leading to improved oxidation resistance and thus showing feasibility. In this work the main focus for development was put on enhancing adhesion and lowering residual stresses of the coatings in order to allow long term and cyclic testing without delamination taking place. Being a very brittle material, Gamma Titanium Aluminides require special surface treatment to enable roughening which is crucial for a strong mechanical bond between substrate and coating. Alternatives to conventional grit blasting as a standard preparation method were investigated. These were micro‐abrasive blasting and blasting at elevated temperature (≈300–550°C) to allow a more ductile behavior. The paper will highlight the implications by means of these measures and will also show the present development status of the multilayer system.     

In Situ Study of γ‐TiAl Lamellae Formation in Supersaturated α2‐Ti3Al Grains

In situ heating transmission electron microscopy (TEM) was used to investigate the initial stage of γ‐TiAl lamellae formation in an intermetallic Ti–45Al–7.5Nb alloy (in at.%). The material was heat treated and quenched in a non‐equilibrium state to consist mainly of supersaturated, ordered α₂‐Ti₃Al grains. Subsequently, specimens were annealed inside a TEM up to 750 °C. The in situ TEM study revealed that ultra‐fine γ‐TiAl laths precipitate in the α₂‐matrix at ≈730 °C which exhibit the classical Blackburn orientation relationship, i.e. (0001)α₂//(111)γ and [$11{\bar {2}}0$ ]α₂//<110]γ. The microstructural development observed in the in situ TEM experiment is compared to results from conventional ex situ TEM studies. In order to investigate the precipitation behavior of the γ‐phase with a complementary method, in situ high energy X‐ray diffraction experiments were performed which confirmed the finding that γ‐laths start to precipitate at ≈730 °C from the supersaturated α₂‐matrix.     

Retransformation (α′→γ) kinetics of strain induced martensite in 304 stainless steel

Coupons of austenitic 304 stainless steel (γ) were transformed to approximately 90% martensite (α′) and 10% austenite by rolling at 77 K. Subsequently the reverse α′→γ transformation was instigated by heating the coupons to 680°C. The retransformation was monitored, in situ, by dilatometry and neutron Bragg edge diffraction (BED). Results from the two techniques show good agreement and suggest that the transformation kinetics are best described by two Avrami exponents, n=2.5 and n=0.2 respectively. A limited discussion of the lattice parameter evolution during the transformation is included. Possible mechanisms for growth dynamics and stress relaxation are discussed.     

Investigation of α platelet boundaries in a near-α titanium alloy

Transmission electron microscopy (TEM) of a bimodal near-α titanium alloy revealed the existence of retained β phase layers and silicide precipitates at the α platelet boundaries inside transformed β grains. The β to α phase transformation accompanied by the precipitation of silicide resulted in the formation of a large number of dislocations at α platelet boundaries. Orientation relationships between silicide, β phase and α phase were also identified. However high-resolution TEM (HRTEM) revealed crystal mismatches between these phases generating high strains at α platelet boundaries. The strengthening effects of the platelet boundaries are discussed in terms of dislocations slip across the boundaries. The mechanism that governs the β to α phase transformation is also discussed.