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International audience; In this work, solid-state a-GeTe growth is studied during the reactive diffusion of a polycrystalline thin film of hexagonal Te deposited on an amorphous Ge thin film (Te-on-Ge) using in situ X-ray diffraction, in situ transmission electron microscopy, and atom probe tomography. After deposition, an amorphous intermixing layer is observed between the Te and Ge layers. a-GeTe is found to form a 2D layer between the deposited Ge and Te layers during growth, with a thickness increasing linearly with time as predicted by the linear-parabolic model for interfacial reaction limited growth. The activation energy of nucleation and interfacial reactions was determined from different isothermal annealing. The obtained results are compared to the observations previously reported during a-GeTe 3D growth in a sample made of an amorphous Ge layer deposited on a polycrystalline Te layer (Ge-on-Te) in the same magnetron sputtering system under the same conditions.

International audience; The effect of Co, Pd and Pt ultrathin films on the kinetics of the formation of Ni-silicide by reactive diffusion is investigated. 50 nm Ni/1 nm X/ 50 nm Ni (X = Co, Pd, Pt) deposited on Si(100) substrates are studied using in-situ and ex-situ measurements by X-ray diffraction (XRD). The presence of Co, Pd or Pt thin films in between the Ni layers delays the formation of the metal rich phase compared to the pure Ni/Si system and thus these films act as diffusion barriers. A simultaneous silicide formation (δ-Ni2Si and NiSi phases) different from the classic sequential formation is found during the consumption of the top Ni layer for which Ni has to diffuse through the barrier. A model for the simultaneous growth in the presence of a barrier is developed, and simulation of the kinetics measured by XRD is used to determine the permeability of the different barriers. Atom probe tomography (APT) of the Ni/Pd/Ni system shows that the Pd layer is located between the Ni top layer and δ-Ni2Si during the silicide growth, in accordance with a silicide formation controlled by Ni diffusion through the Pd layer. The effect of the barrier on the silicide formation and properties is discussed.

International audience; The properties of oxide dispersion-strengthened steels are highly dependent on the nature and size distribution of their constituting nano-oxide precipitates. A fine control of the processes of synthesis would enable the optimization of pertinent properties for use in various energy systems. This control, however, requires knowledge of the precise mechanisms of nucleation and growth of the nanoprecipitates, which are still a matter of debate. In the present study, nano-oxide precipitates were produced via the implantation of Y, Ti, and O ions in two different sequential orders in an Fe-10%Cr matrix that was subsequently thermally annealed. The results show that the oxides that precipitate are not necessarily favoured thermodynamically, but rather result from complex kinetics aspects related to the interaction between the implanted elements and induced defects. When Y is implanted first, the formation of nanoprecipitates with characteristics similar to those in conventionally produced ODS steels, especially with a core/shell structure, is evidenced. In contrast, when implantation starts with Ti, the precipitation of yttria during subsequent high-temperature annealing is totally suppressed, and corundum Cr2O3 precipitates instead. Moreover, the systematic involvement of {110} matrix planes in orientation relationships with the precipitates, independently of the precipitate nature, suggests matrix restriction effects on the early stages of precipitation.

International audience; The compound GeTe, despite its simple stoichiometry, is rather unconventional and has been investigated both from a fundamental and technological perspective: it is of high interest for several technologies such as data-storage (phase change memories) and thermoelectricity. The understanding of GeTe growth is thus a key issue for technological applications and fundamental understanding. In this work, GeTe crystallization kinetics is compared to Ge/Te reactive diffusion kinetics using in situ X-ray diffraction measurements, as well as in situ transmission electron microscopy. GeTe crystallization from an amorphous solid solution exhibiting the stoichiometry of the compound GeTe is found to occur at the same temperature as for the reactive diffusion of an amorphous Ge layer on top of a polycrystalline Te layer. Furthermore, GeTe growth is of tridimensional type in the two cases, and can be modeled by the Johnson-Mehl-Avrami-Kolmogorov model. Using this model, the activation energies of nucleation and growth were determined for both crystallization and reactive diffusion. The results suggest that GeTe exhibits nucleation/reaction kinetics unusually low compared to atomic transport kinetics, contrasting with other germanides.

The nanometer-scale (nano-scale) microstructural evolution in an additively manufactured Re-free Ni-based superalloy, with single crystal compositions, is investigated through field emission scanning electron microscopy, transmission electron microscopy, and atom probe tomography. We find that nano-scale primary γ′ precipitation occurs in the fine as-built microstructure, leading to an exceptional microhardness of 480.0 ± 6.7 HV at room temperature. Presence of ultra-fine γ′ precipitates, ~ 20 nm in size, is observed in the bottom few layers of the as-built samples, which is hitherto undocumented and contrary to the widespread consensus regarding hierarchical γ′ phase evolution in additively manufactured Ni-based superalloys. Moreover, considerable precipitation of tantalum-rich C14 Laves phase at the grain boundaries and interdendritic regions in the as-built samples emphasizes the need for additive manufacturing specific alloy design. National Research Foundation (NRF) Accepted version

The semi-conductor Ge1―xSnx exhibits interesting properties for optoelectronic applications. In particular, Ge1―xSnx alloys with x ≥ 0.1 exhibit a direct band-gap, and integrated in complementary-metal-oxide-semiconductor (CMOS) technology, should allow the development of Si photonics. CMOS-compatible magnetron sputtering deposition was shown to produce monocrystalline Ge1―xSnx films with good electrical properties at low cost. However, these layers were grown at low temperature ( 600 K) on Si(001) by magnetron sputtering in order to produce low-cost and CMOS-compatible relaxed pseudo-coherent layers with x ≥ 0.1 exhibiting a better crystallinity. Ge1―xSnx crystallization and Ge1―xSnx crystal growth were investigated. Crystallization of an amorphous Ge1―xSnx layer deposited on Si(001) or Ge(001) grown on Si(001) leads to the growth of polycrystalline films. Furthermore, the competition between Ge/Sn phase separation and Ge1―xSnx growth prevents the formation of large-grain Sn-rich Ge1―xSnx layers without the formation of β-Sn islands on the layer surface, due to significant atomic redistribution kinetics at the crystallization temperature (T = 733 K for x = 0.17). However, the growth at T = 633 K of a highly-relaxed pseudo-coherent Ge0.9Sn0.1 film with low impurity concentrations (

International audience; In the galvannealing process, steel strips are immersed in molten zinc containing 0.100 to 0.135 wt pct Al at 450°C. The coating obtained is composed of a thin intermetallic compounds' layer called the inhibition layer (200 nm) covered with a thick zinc layer (10 lm). The nature of this inhibition layer has been investigated here for a galvanizing bath with a low Al content. The inhibition layer formed on industrial low-alloyed steels was characterized by transmission electron microscopy and atom probe tomography. The inhibition layer is composed of a thin Fe 2 Al 5 Zn x layer (20 nm), covered with a thicker d layer (200 nm). The Fe 2 Al 5 Zn x layer is discontinuous at the lowest bath Al content. Small precipitates (20 nm in diameter) with a stoichiometry corresponding to Fe 3 Al-containing Zn were also found for the first time in the d phase. The microstructure of the inhibition layer can be described with diffusion paths drawn in the Al-Fe-Zn ternary section at 450°C. This means that all interfaces of the inhibition layer are at thermodynamic equilibrium. The Fe 2 Al 5 Zn x layer is formed on the steel surface before the d layer. The nucleation and growth of the Fe 3 Al-Zn particles probably occur in the liquid metal at the same time as d.

PdGe contact fabrication on Ge(001) wafers doped with Ga is investigated using conventional complementary metal-oxide-semiconductor processes. Despite a p-type doping level of ~1.4 × 1020 cm−3, the resistivity of the PdGe contact is found to be twice higher than that of undoped Ge. Ga doping has no influence on the Pd reaction with Ge. However, the doping process and the Salicide process led to the formation of Ga-Pd defects in both sides of the PdGe/Ge interface, resulting from Ga and Pd co-segregation on Ge dislocation loops.

International audience; Mg-Ag-Sb thin films were deposited by magnetron sputtering using a commercial Mg 1/3 Ag 1/3 Sb 1/3 target. All the films contain principally the two phases Ag 3 Sb and alpha-MgAgSb in same proportions but exhibit different microstructures. The films have the same Seebeck coefficient despite the difference of interface density and structure. Theoretical calculations show that the film effective Seebeck coefficient S is depending only on the volume of each phase present in the film and their Seebeck coefficients. The multiple interfaces between the different phases have no effect on S .

Carbon-doped Mn5Ge3 thin films were grown using magnetron sputtering and reactive diffusion or non-diffusive reaction (NDR). The C content, the Curie temperature, and the resonance field difference between the hard and easy axis were measured for all the films, allowing linear relations between these three parameters to be quantitatively determined. Thanks to these functions, the measurement of a single of these parameters allows the two others to be known. The association of the sputtering technique to the NDR process appears as the best way for producing C-doped Mn5Ge3 thin films.

20th International Conference on Composite Materials (ICCM), Copenhagen, DENMARK, JUL 24-28, 2015; International audience; The mechanical properties of precipitation-hardened stainless steels rely on a complex multi-scale microstructure developed during a sequence of quenching after austenitization, followed by a precipitation heat treatment. Important features of the resulting microstructure include the microstructure of martensite, retained and reverted austenite, nanoscale precipitation and the homogeneity of the Cr concentration. In this paper, the microstructure of a Cu-bearing 15-5PH steel is thoroughly characterized along the precipitation heat treatment, using a combination of transmission electron microscopy with phase and orientation mapping, atom probe tomography, in-situ small-angle X-ray scattering and X-ray diffraction. The fraction of austenite is observed to increase during the ageing treatment, together with the precipitation of the Cu precipitates, which present a core-shell structure with a shell enriched in Ni, Mn and Si. After heat treatment, the Cr concentration is found to be slightly inhomogeneous in the matrix, with some segregations at the dislocations. (C) 2016 Elsevier Ltd. All rights reserved.

International audience; One major hindrance that alloy design for additive manufacturing (AM) faces nowadays is hot tearing. Contrary to the previous works which either try to reduce solidification range or introduce grain refinement, the current work presents a new approach of employing segregation engineering to alter the residual stress states at the interdendritic and grain boundary regions and consequently prevent hot tearing. Here, in situ Al alloying is introduced into an existing hot-cracking susceptible high-entropy alloy CoCrFeNi. It is found that within a certain range of compositions, such as Al0.5CoCrFeNi, the hot crack density was drastically decreased. During the solidification of this specific alloy composition, Al is firstly ejected from the primary dendritic face-centred cubic (FCC) phase and segregates into the interdendritic regions. Spinodal decomposition then occurs in these Al-enriched regions to form the ordered B2 NiAl and disordered body-centred cubic (BCC) Cr phases. Due to the higher molar volume and lower homologous temperatures of these B2/BCC phases, the inherent residual strain is accommodated and transformed from a maximum 0.006 tensile strain in CoCrFeNi to a compressive strain of ~0.001 in Al0.5CoCrFeNi. It is believed that this grain boundary segregation engineering method could provide a new pathway to systematically counteract the hot tearing problem in additive manufacturing of metals and alloys, using available thermodynamic and kinetic database information.

Hot tearing mechanisms of a high-entropy alloy CoCrFeNi additively manufactured by selective laser melting have been investigated. Intergranular hot cracks are present regardless of various parameters used, suggesting poor laser-based printability for the alloy. Elemental segregation does not exist at the grain boundary that favours the hot cracking. We find that severe residual stress induced by the large grain size is the root cause for the intergranular cracking. The classic Rappaz-Drezet-Gremaud model is used to predict the characteristic depression pressure limit beyond which hot tearing will occur for the selective laser melting of metals and alloys. National Research Foundation (NRF) Accepted version The authors are grateful for the use of resources in Singapore Centre for 3D Printing funded by the Singapore National Research Foundation (NRF).

International audience; Ion irradiations on the Ti6-4 titanium alloy were conducted at the JANNUS French platform in two different conditions of temperatures, doses and fluxes, to simulate neutron irradiation damage. Quantification of defects and chemical microanalyses were carried out thanks to Transmission Electron Microscopy and Atom Probe Tomography. -type loops and radiation induced precipitates (a vanadium-rich β BCC phase) were observed for both irradiation temperatures. During an irradiation at 300 °C, there was no notable influence of the dose and flux for the considered doses and fluxes ranges on the -type defects. The influence of raising the irradiation temperature up to 430 °C was a lowering of their density and an increase of their mean diameter for both defects. In addition, a lower flux seemed to enhance this temperature effect. These phenomena were very significant for precipitates whereas it appeared very modest for -type loops. The probable mechanism to explain the distribution of vanadium-rich β precipitates inside the α phase is the heterogeneous nucleation. The nucleation is dominated by the Radiation Induced Segregation (RIS) phenomenon at 430 °C and could be dominated by the mechanism of vanadium-rich clusters formation by ballistic effects in the cascades at 300 °C.

Self-diffusion experiments in single crystalline isotopically controlled silicon nanowires with diameters of 70 and 400 nm at 850 and 1000 °C are reported. The isotope structures were first epitaxially grown on top of silicon substrate wafers. Nanowires were subsequently fabricated using a nanosphere lithography process in combination with inductively coupled plasma dry reactive ion etching. Three-dimensional profiling of the nanosized structure before and after diffusion annealing was performed by means of atom probe tomography (APT). Self-diffusion profiles obtained from APT analyses are accurately described by Fick's law for self-diffusion. Data obtained for silicon self-diffusion in nanowires are equal to the results reported for bulk silicon crystals, i.e., finite size effects and high surface-to-volume ratios do not significantly affect silicon self-diffusion. This shows that the properties of native point defects determined from self-diffusion in bulk crystals also hold for nanosized silicon structures with diameters down to 70 nm.Self-diffusion experiments in single crystalline isotopically controlled silicon nanowires with diameters of 70 and 400 nm at 850 and 1000 °C are reported. The isotope structures were first epitaxially grown on top of silicon substrate wafers. Nanowires were subsequently fabricated using a nanosphere lithography process in combination with inductively coupled plasma dry reactive ion etching. Three-dimensional profiling of the nanosized structure before and after diffusion annealing was performed by means of atom probe tomography (APT). Self-diffusion profiles obtained from APT analyses are accurately described by Fick's law for self-diffusion. Data obtained for silicon self-diffusion in nanowires are equal to the results reported for bulk silicon crystals, i.e., finite size effects and high surface-to-volume ratios do not significantly affect silicon self-diffusion. This shows that the properties of native point defects determined from self-diffusion in bulk crystals also hold for nanosized silicon struc...

Electron beam melting (EBM®)-built Ti–6Al–4V has increasingly shown great potential for orthopedic implant and aerospace applications in recent years. The microstructure and mechanical properties of EBM-built Ti–6Al–4V have been systematically investigated in this work. Its microstructure consists of columnar prior β grains delineated by wavy grain boundary α and transformed α/β structures with both cellular colony and basket-weave morphology as well as numerous singular α bulges within the prior β grains. The β phase is found to form as discrete flat rods embedded in continuous α phase and its volume fraction is determined to be ∼3.6%. Moreover, α′ martensite was not observed as it has decomposed into α and β phases. In particular, the α/β interface was studied in detail combined transmission electron microscopy with atom probe tomography. Of note is that graded Ti–6Al–4V microstructure i.e. both prior β grain width and β phase interspacing continuously increase with the build height, was observed, which mainly arises from the decreasing cooling rate. Furthermore, an increasingly pronounced strain hardening effect was also observed as the previously built layers undergo a longer annealing compared to the subsequent layers. As a result, graded mechanical properties of Ti–6Al–4V with degraded microhardness and tensile properties were found. A good agreement with the Hall–Petch relation indicates that the graded property takes place mainly due to the graded microstructure. In addition, this graded microstructure and mechanical properties were discussed based on a quantitative characterization.

A combinatorial study of the combined effect of Pt and W on Ni silicide formation is performed. Ni(Pt, W) films with thickness and composition gradients were prepared by a co-deposition composition spread technique using sputtering deposition from Pt, W, and Ni targets. The deposited Ni(Pt,W) films were characterized by X-ray diffraction, X-ray reflectivity, Rutherford backscattering, and atom probe tomography. The maximum content of alloying elements is close to 27 at. %. Simulations of the thickness and composition were carried out and compared with experimental results. In situ X-ray diffraction and atom probe tomography were used to study the phase formation. Both additive alloying elements (Pt + W) slow down the Ni consumption and the effect of W is more pronounced than the one of Pt. Regarding the effect of alloying elements on Ni silicides formation, three regions could be distinguished in the Ni(Pt,W)/Si wafer. For the region close to the Ni target, the low contents of alloying elements (Pt + W) have little impact on the phase sequence (δ-Ni2Si is the first silicide and NiSi forms when Ni is entirely consumed) but the kinetics of silicide formation slows down. The region close to the Pt target has high contents of (Pt + W) and is rich in Pt and a simultaneous phase formation of δ-Ni2Si and NiSi is observed. For the high (Pt + W) contents and W-rich region, NiSi forms unexpectedly before δ-Ni2Si and the subsequent growth of δ-Ni2Si is accompanied by the NiSi consumption. When Ni is entirely consumed, NiSi regrows at the expense of δ-Ni2Si.A combinatorial study of the combined effect of Pt and W on Ni silicide formation is performed. Ni(Pt, W) films with thickness and composition gradients were prepared by a co-deposition composition spread technique using sputtering deposition from Pt, W, and Ni targets. The deposited Ni(Pt,W) films were characterized by X-ray diffraction, X-ray reflectivity, Rutherford backscattering, and atom probe tomography. The maximum content of alloying elements is close to 27 at. %. Simulations of the thickness and composition were carried out and compared with experimental results. In situ X-ray diffraction and atom probe tomography were used to study the phase formation. Both additive alloying elements (Pt + W) slow down the Ni consumption and the effect of W is more pronounced than the one of Pt. Regarding the effect of alloying elements on Ni silicides formation, three regions could be distinguished in the Ni(Pt,W)/Si wafer. For the region close to the Ni target, the low contents of alloying elements (Pt + W) h...

To enhance the morphological stability of NiGe, a material of interest as a source drain-contact in Ge-based field effect transistors, Ta or W, is added as either an interlayer or a capping layer. The efficacy of this Ta or W addition is evaluated with pure NiGe as a reference. While interlayers increase the NiGe formation temperature, capping layers do not retard the NiGe formation. Regardless of the initial position of Ta or W, the morphological stability of NiGe against agglomeration can be improved by up to 100 °C. The improved thermal stability can be ascribed to an inhibited surface diffusion, owing to Ta or W being located on top of NiGe after annealing, as confirmed by means of transmission electron microscopy, Rutherford backscattering spectrometry, and atom probe tomography. The latter also shows a 0.3 €‰at. % solubility of Ta in NiGe at 450 °C, while no such incorporation of W is detectable.

Carbide precipitation plays a key role in determining mechanical properties of Co-Cr-Mo alloy. Precipitation characteristics of carbides in selective electron beam melting (SEBM)-fabricated Co-Cr-Mo parts have been investigated by atom probe tomography and transmission electron microscopy. We observe co-existence of two types of carbides, i.e. M23C6 and M6C, which are formed into continuous carbide thin films along columnar grain boundaries. The carbide thin film is found to precipitate coherently with one γ Co grain while incoherently with another adjacent one. Moreover, columnar carbide chains or clusters consisting of nanometer-sized, cuboidal particles are precipitated coherently with surrounding γ Co phase within interdendritic regions.

International audience; PdGe contact fabrication on Se-doped Ge(001) is investigated. PdGe thin film resistivity is two times lower if the PdGe layer is grown by Pd reactive diffusion on Se-doped Ge, compared to PdGe layer grown in the same condition on Se-free Ge. The phase sequence and the phase growth kinetics during Pd reactive diffusion with Ge are not modified by the presence of Se atoms. However, the PdGe film texture is different with Se, and Se segregates at the PdGe/Ge interface. These results suggest that Se atoms may be used to produce efficient contacts on n-type Ge. (c) 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

International audience; An improved nanofabrication processing technique for realization of vertically aligned silicon nanowires (SiNW5) by colloidal lithography is reported in this work. Microstructure pattern arrays are prepared on the substrate allowing selective deposition of polystyrene (PS) nanoparticles. Using PSS/PDDA/PSS-layer, surface properties can be modified resulting in an enhanced hydrophilicity of the silicon substrate, which is followed by high surface coverage up to-83% after particle transfer. During the fabrication, we demonstrate full control of the mask dimension providing excellent control of nanostructure feature size by inductively coupled plasma (ICP) reactive ion etching (RIE) process at cryogenic temperature. Finally, this combined approach of bottom-up and top-down methods offers simple and direct nanoscale processing steps with low-cost and great reproducibility, enabling high density fabrication of nanostructure (similar to 10(9) SiNW/cm(2)) within certain area. This preparation route of the SiNWs was applied to isotopically controlled silicon layers grown epitaxially on Si substrates. Atom probe tomography of these SiNWs reveal that the isotope layer ordering is preserved by the NW fabrication route. (C) 2017 Elsevier B.V. All rights reserved.

At high temperatures under oxidizing environments, titanium-based alloys form an oxide scale and dissolve large amount of oxygen in their metallic matrix. Oxygen dissolution is a cause of embrittlement. Nitrogen is a secondary oxidant, which also dissolves in titanium during oxidation in air. Oxidation experiments of Ti-6Al-2Sn-4Zr-2Mo-0.1Si titanium-based alloy at 650 °C for 1000 h in synthetic air (20%O2- 80%N2) and in a mixture of 20%O2-80%Ar, showed that nitrogen reduces both oxide scale growth and oxygen dissolution. Atom probe tomography revealed that nitrogen effect is due to the formation of an interfacial layer of nitride Ti2N but also to the formation of a nitrogen rich a-Ti-based solid solution, which both act as difiusion barriers for oxygen because of their low oxygen solubility.

Ni silicides used as contacts in source/drain and gate of advanced CMOS devices were analyzed by atom probe tomography (APT) at atomic scale. These measurements were performed on 45 nm nMOS after standard self-aligned silicide (salicide) process using Ni(5 at.% Pt) alloy. After the first annealing (RTA1), δ-Ni 2 Si was the only phase formed on gate and source/drain while, after the second annealing (RTA2), two different Ni silicides have been formed: NiSi on the gate and δ-Ni 2 Si on the source and drain. This difference between source/drain and gate regions in nMOS devices has been related to the Si substrate nature (poly or mono-crystalline) and to the size of the contact. In fact, NiSi seems to have difficulties to nucleate in the narrow source/drain contact on mono-crystalline Si. The results have been compared to analysis performed on 28 nm nMOS where the Pt concentration is higher (10 at.% Pt). In this case, θ-Ni 2 Si is the first phase to form after RTA1 and NiSi is then formed at the same time on source (or drain) and gate after RTA2. The absence of the formation of NiSi from δ-Ni 2 Si/Si(1 0 0) interface compared to θ-Ni 2 Si/Si(1 0 0) interface could be related to the difference of the interface energies. The redistributions of As and Pt in different silicides and interfaces were measured and discussed. In particular, it has been evidenced that Pt redistributions obtained on both 45 and 28 nm MOS transistors correspond to respective Pt distributions measured on blanket wafers.

In microelectronics, the increase in complexity and the reduction of devices dimensions make essential the development of new characterization tools and methodologies. Indeed advanced characterization methods with very high spatial resolution are needed to analyze the redistribution at the nanoscale in devices and interconnections. The atom probe tomography has become an essential analysis to study materials at the nanometer scale. This instrument is the only analytical microscope capable to produce 3D maps of the distribution of the chemical species with an atomic resolution inside a material. This technique has benefit from several instrumental improvements during last years. In particular, the use of laser for the analysis of semiconductors and insulating materials offers new perspectives for characterization. The capability of APT to map out elements at the atomic scale with high sensitivity in devices meets the characterization requirements of semiconductor devices such as the determination of elemental distributions for each device region. In this paper, several examples will show how APT can be used to characterize and understand materials and process for advanced metallization. The possibilities and performances of APT (chemical analysis of all the elements, atomic resolution, planes determination, crystallographic information…) will be described as well as some of its limitations (sample preparation, complex evaporation, detection limit, …). The examples illustrate different aspect of metallization: dopant profiling and clustering, metallic impurities segregation on dislocation, silicide formation and alloying, high K/metal gate optimization, SiGe quantum dots, as well as analysis of transistors and nanowires.

Metallic silicides have been used as contact materials on source/drain and gate in metal-oxide semiconductor (MOS) structure for 40 years. Since the 65 nm technology node, NiSi is the preferred material for contact in microelectronic due to low resistivity, low thermal budget, and low Si consumption. Ni(Pt)Si with 10 at.% Pt is currently employed in recent technologies since Pt allows to stabilize NiSi at high temperature. The presence of Pt and the very low thickness (

A ZnSe layer grown on a GaAs substrate by molecular beam epitaxy has been analysed by atom probe tomography. The one-dimensional concentration profile shows separation between Zn and Se and between Ga and As at the interface. A comparison of the concentration profile with different interface models suggests that the formation of a Ga 2 + x Se 3 compound at the ZnSe/GaAs interface with fewer vacancies than Ga 2 Se 3 ( x = 0.7). These results show the ability of atom probe tomography to characterize the interface at the atomic scale.

The redistribution of arsenic and nickel during the reaction of Ni thin films with arsenic doped Si(100) substrates is studied by a combination of transmission electron microscopy (TEM), atom-probe tomography (APT) and in situ X-ray diffraction (XRD). Ni was observed at the edges of a pseudo-hexagonal dislocation loop within As^+-implanted (001)Si wafers, after recrystallisation of preamorphised Si and deposition of 100nm Ni. After an additional heat treatment at 280^oC, the same concentration profiles were found with a maximum of ~10% Ni at the edges of the dislocation loops, suggesting Cottrell atmospheres. In situ XRD showed the formation of a transient phase forming isolated grains at the @d-Ni"2Si/Si interface. Clusters containing 10% of As are present only in the transient phase. The presence of As clusters in silicide used for contact on devices might have significant influences on devices properties.

International audience; The microstructure of a 6061-T6 Al alloy subjected to ion irradiation at 95 and 165 displacements per atom (dpa) has been evaluated by transmission electron microscopy and atom-probe tomography. The initial microstructure of the alloy is dominated by needle-shaped β″ precipitates. After 95 dpa irradiation, the β″ precipitates display a slight lattice distortion and are partially dissolved, together with the formation of a new phase. After 165 dpa irradiation, the β″ precipitates are completely dissolved, the new phase has grown and a high density of clusters rich in Mg, Si, Cu and Cr is observed. The determination of ballistic versus radiation enhanced diffusion coefficients shows that enhanced diffusion is predominant for β” dissolution. The formation and growth of the new particles may be caused by radiation induced segregation. Solute drag by vacancies or mixed dumbbell interstitials migration could explain the diffusion of some elements as Si or Cr towards the new particles.

International audience; Oxide dispersion strengthened (ODS) steels are promising structural materials for the next generation nuclear reactors, as well as fusion facilities. The detailed understanding of the mechanisms involved in the precipitation of nano-oxides during ODS steel production would strongly contribute to the improvement of the mechanical properties and the optimization of manufacturing of ODS steels, with a potentially strong economic impact for their industrialization. A useful tool for the experimental study of nano-oxide precipitation is ion implantation, a technique that is widely used to synthesize precipitate nanostructures in well-controlled conditions. Earlier, we have demonstrated the feasibility of synthesizing aluminum-oxide particles in the high purity Fe-10Cr alloy by consecutive implantation with Al and O ions at room temperature. This paper describes the effects of high-temperature annealing after the ion implantation stage on the development of the aluminum based oxide nanoparticle system. Using transmission electron microscopy and atom probe tomography experiments, we demonstrate that post-implantation heat treatment induces the growth of the nano-sized oxides in the implanted region and nucleation of new oxide precipitates behind the implantation zone as a result of the diffusion driven broadening of implant profiles. A tentative scenario for the development of metal-oxide nano-particles at both ion implantation and heat treatment stages is suggested based on the experimental observations.

The unique capabilities of atom probe tomography (APT) to characterize internal interfaces and layer chemistry with sub-nanometer scale resolution in three dimensions have been recently opened up to materials with poor electrical conductivity by the use of ultrafast laser pulses. The progress in sample preparation (focused ion beam) as well as in instrument performance enable now the analysis of relatively large volumes with typical diameters of 100 to 200 nm and depths of several hundred nm (this corresponds to an increase by several order of magnitude compared to the former instrument) of site specific samples. In this work, APT is used to study the effects of Pt on the formation and stability of Ni silicides. The precise location of this alloy element has been determined at the nanometer scale: In particular, APT allows us to quantify the amount of Pt in the grain boundaries (GB) of Ni2Si for about 100 different grain boundaries and thus to better characterize the GB diffusion and segregation.

As an important metal three-dimensional printing technology, electron beam melting (EBM) is gaining increasing attention due to its huge potential applications in aerospace and biomedical fields. EBM processing of Ti-6Al-4V as well as its microstructure and mechanical properties were extensively investigated. However, it is still lack of quantitative studies regarding its microstructural evolution, indicative of EBM thermal process. Here, we report α′ martensitic transformation and α/β interface evolution in varied printing thicknesses of EBM-printed Ti-6Al-4V block samples by means of atom probe tomography. Quantitative chemical composition analysis suggests a general phase transformation sequence. By increasing in-fill hatched thickness, elemental partitioning ratios arise and β volume fraction is increased. Furthermore, we observe kinetic vanadium segregation and aluminum depletion at interface front and the resultant α/β interface widening phenomenon. It may give rise to an increased α/β lattice mismatch and weakened α/β interfaces, which could account for the degraded strength as printing thickness increases. NRF (Natl Research Foundation, S’pore) ASTAR (Agency for Sci., Tech. and Research, S’pore) Published version

International audience; The microstructure and the solute distribution inside the phases after isothermal holding in the temperature range between 420°C and 700°C in the Ti-5553 alloy were analyzed using TEM equipped with an EDX analyzer and atom probe tomography. When phase transformation occurred at high temperatures (≥ 600°C), a significant partitioning of all solute elements was characterized. After a long holding time, the distribution was nearly homogeneous in each phase. For a transformation at lower temperature (410°C), a low partitioning was observed at the beginning of the transformation, after 40 min, and the precipitates composition notably evolved with increasing time toward an expected composition of equilibrium alpha phase.

In situ sheet resistance and x-ray diffraction measurements were used simultaneously during heat treatment to study Ti electrodes in contact with Ge-Te phase change materials. Ti is found to react with GeTe forming TiTe 2 and Ge. Atom probe tomography analyses confirm the presence of these two phases after a 400°C heat treatment.

The Ni silicide formed at low temperature on Si nanowire has been analyzed by atom probe tomography (APT) thanks to a special technique for sample preparation. A method of preparation has been developed using the focused ion beam (FIB) for the APT analysis of nanowires (NWs). This method allow for the measurement of the radial distribution when a NW is cut, buried in a protective metal matrix, and finally mounted on the APT support post. This method was used for phosphorous doped Si NWs with or without a silicide shell, and allows obtaining the concentration and distribution of chemical elements in three-dimensions (3D) in the radial direction of the NWs. The distribution of atoms in the NWs has been measured including dopants and Au contamination. These measurements show that δ-Ni2Si phase is formed on Si NW, Au is found as cluster at the Ni/δ-Ni2Si interface and P is segregated at the δ-Ni2Si/ Si NW interface. The results obtained on NWs after silicidation were compared with the silicide on the Si substrate, showing that the same silicide phase δ-Ni2Si formed in both cases (NWs and substrate).

International audience; This paper reports the feasibility of nano-oxide precipitate formation in Fe-Cr alloy by ion implantation synthesis. High contents of Al+ and O+ ions were implanted into thin films of high purity Fe-10%Cr alloy at room temperature and were studied by transmission electron microscopy (TEM) and atom probe tomography (APT). In contrast, to the common two-stage implantation/annealing scheme of precipitate ensemble synthesis by ion beams, cluster formation took place at the implantation stage in our study, requiring no subsequent high-temperature annealing. The post-implantation microstructural examination revealed in the as-implanted thin foil an array of precipitates with diameters in the range of 3-30 nm. The precipitate number density distribution was found to depend on the foil thickness. The precipitate enrichment with both Al and O was confirmed by the energy-filtered TEM analysis. Judging from the electron diffraction pattern and high-resolution TEM analysis, the crystal lattice of precipitates corresponds to some cubic modification of aluminium-rich oxide or pure aluminium oxide. The precipitate lattice alignment with the host matrix was revealed for at least a part of precipitates. The analysis of APT data using cluster detection algorithm indicates the presence of local zones enriched in Al and O, even in those areas of as-implanted samples where no clusters were visible by TEM.

International audience; The monolithic integration of III-V semiconductors on silicon and particularly of GaAs has aroused great interest since the 1980s. Potential applications are legion, ranging from photovoltaics to high mobility channel transistors. By using a novel integration method, we have shown that it is possible to achieve heteroepitaxial integration of GaAs crystals (typical size 1 lm) on silicon without any structural defect such as antiphase domains, dislocations, or stress, usually reported for direct GaAs heteroepitaxy on silicon. However, concerning their electronic properties, conventional free carrier characterization methods are impractical due to the micrometric size of GaAs crystals. In order to evaluate the GaAs material quality for optoelectronic applications, a series of indirect analyses such as atom probe tomography, Raman spectroscopy, and micro-photoluminescence as a function of temperature were performed. These revealed a high content of partially electrically active carbon originating from the trimethylgallium used as the Ga precursor. Nevertheless, the very good homogeneity observed by this doping mechanism and the attractive properties of carbon as a dopant once controlled to a sufficient degree are a promising route to device doping.

The formation of Ni silicide alloyed with Pt has been analyzed by atom probe tomography. A 300 °C/1 h anneal results in simultaneous growth of the NiSi and Ni 2 Si phases: the Ni 2 Si phase is a continuous layer with columnar grains, while the NiSi phase forms a discontinuous layer. Direct evidence of Pt diffusion short-circuits via Ni 2 Si grain boundaries is shown. The presence of Pt in the grains and interphase boundaries may explain the change in the Ni silicide formation for the Ni(5% Pt)/Si system.

The flow of hydrogen, helium, and nitrogen through a millimeter long and micrometer size annulus capillary from a high pressure chamber to a low pressure chamber is measured in a wide pressure range. The corresponding gas conductance is deduced. Molecular, transition, and viscous regimes are observed. The local supply of gas strongly increases with pressure in the viscous regime up to a regime controlled by capillary exit loss. Based on such a geometry, the gas supply to a field ion source with a coaxial structure is shown to be increased by more than three orders of magnitude compared to a conventional supply.