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At least 1,207 records · Page 67
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DOE OSTI2014

Chemical delithiation and exfoliation of Li{sub x}CoO{sub 2}

Progressive chemical .delithiation of commercially available lithium cobalt oxide (LiCoO{sub 2}) showed consecutive changes in the crystal properties. Rietveld refinement of high resolution X-ray and neutron diffraction revealed an increased lattice parameter c and a reduced lattice parameter a for chemically delithiated samples. Using electron microscopy we have also followed the changes in the texture of the samples towards what we have found is a critical layer stoichiometry of about Li{sub x}CoO{sub 2} with x=1/3 that causes the grains to exfoliate. The pattern of etches by delithiation suggests that unrelieved strain fields may produce chemical activity. - Graphical abstract: The effect of chemical dedoping of Li{sub x}CoO{sub 2} leads to a significant change in the (003) peak and to exfoliation for x=1/3. - Highlights: • Chemical delithiation of Li{sub x}CoO{sub 2} showed consecutive changes in crystal properties. • We performed X-ray as well as neutron diffraction on delithiated material. • Crystal analysis revealed an increased c and a reduced a for delithiated samples. • Electron microscopy revealed changes in the texture for Li{sub x}CoO{sub 2} (x=1/3)

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Effect of synthesis methods on the Ca{sub 3}Co{sub 4}O{sub 9} thermoelectric ceramic performances

Three different synthesis methods producing nanometric grain sizes, coprecipitation with ammonium carbonate, oxalic acid, and by attrition milling have been studied to produce Ca{sub 3}Co{sub 4}O{sub 9} ceramics and compared with the classical solid state route. These three processes have produced high reactive precursors and all the organic material and CaCO{sub 3}·have been decomposed in a single thermal treatment. Coprecipitation leads to pure Ca{sub 3}Co{sub 4}O{sub 9} phase, while attrition milling and classical solid state produce small amounts of Ca{sub 3}Co{sub 2}O{sub 6} secondary phase. Power factor values are similar for all three samples, being slightly lower for the ones produced by attrition milling. These values are much higher than the obtained in samples prepared by the classical solid state method, used as reference. The maximum power factor values determined at 800 °C (∼0.43 mW/K{sup 2} m) are slightly higher than the best reported values obtained in textured ones which also show much higher density values. - Graphical abstract: Impressive raise of PF in Ca{sub 3}Co{sub 4}O{sub 9} thermoelectric materials obtained from nanometric grains. - Highlights: • Ca{sub 3}Co{sub 4}O{sub 9} has been produced by four different methods. • Precursors particle sizes influences on the final performances. • Coprecipitation methods produce single Ca{sub 3}Co{sub 4}O{sub 9} phase. • Power factor reaches values comparable to high density textured materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Determining the sputter yields of molybdenum in low-index crystal planes via electron backscattered diffraction, focused ion beam and atomic force microscope

Previous literature has used several monocrystalline sputtering targets with various crystalline planes, respectively, to investigate the variations of the sputter yield of materials in different crystalline orientations. This study presents a method to measure the sputtered yields of Mo for the three low-index planes (100), (110), and (111), through using an easily made polycrystalline target. The procedure was firstly to use electron backscattered diffraction to identify the grain positions of the three crystalline planes, and then use a focused ion beam to perform the micro-milling of each identified grain, and finally the sputter yields were calculated from the removed volumes, which were measured by atomic force microscope. Experimental results showed that the sputter yield of the primary orientations for Mo varied as Y{sub (110)} > Y{sub (100)} > Y{sub (111)}, coincidental with the ranking of their planar atomic packing densities. The concept of transparency of ion in the crystalline substance was applied to elucidate these results. In addition, the result of (110) orientation exhibiting higher sputter yield is helpful for us to develop a Mo target with a higher deposition rate for use in industry. By changing the deformation process from straight rolling to cross rolling, the (110) texture intensity of the Mo target was significantly improved, and thus enhanced the deposition rate. - Highlights: • We used EBSD, FIB and AFM to measure the sputter yields of Mo in low-index planes. • The sputter yield of the primary orientations for Mo varied as Y{sub (110)} > Y{sub (100)} > Y{sub (111)}. • The transparency of ion was used to elucidate the differences in the sputter yield. • We improved the sputter rate of polycrystalline Mo target by adjusting its texture.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Precipitation in cold-rolled Al–Sc–Zr and Al–Mn–Sc–Zr alloys prepared by powder metallurgy

The effects of cold-rolling on thermal, mechanical and electrical properties, microstructure and recrystallization behaviour of the AlScZr and AlMnScZr alloys prepared by powder metallurgy were studied. The powder was produced by atomising in argon with 1% oxygen and then consolidated by hot extrusion at 350 °C. The electrical resistometry and microhardness together with differential scanning calorimetry measurements were compared with microstructure development observed by transmission and scanning electron microscopy, X-ray diffraction and electron backscatter diffraction. Fine (sub)grain structure developed and fine coherent Al{sub 3}Sc and/or Al{sub 3}(Sc,Zr) particles precipitated during extrusion at 350 °C in the alloys studied. Additional precipitation of the Al{sub 3}Sc and/or Al{sub 3}(Sc,Zr) particles and/or their coarsening was slightly facilitated by the previous cold rolling. The presence of Sc,Zr-containing particles has a significant antirecrystallization effect that prevents recrystallization at temperatures minimally up to 420 °C. The precipitation of the Al{sub 6}Mn- and/or Al{sub 6}(Mn,Fe) particles of a size ∼ 1.0 μm at subgrain boundaries has also an essential antirecrystallization effect and totally suppresses recrystallization during 32 h long annealing at 550 °C. The texture development of the alloys seems to be affected by high solid solution strengthening by Mn. The precipitation of the Mn-containing alloy is highly enhanced by a cold rolling. The apparent activation energy of the Al{sub 3}Sc particles formation and/or coarsening and that of the Al{sub 6}Mn and/or Al{sub 6}(Mn,Fe) particle precipitation in the powder and in the compacted alloys were determined. The cold deformation has no effect on the apparent activation energy values of the Al{sub 3}Sc-phase and the Al{sub 6}Mn-phase precipitation. - Highlights: • The Mn, Sc and Zr additions to Al totally suppresses recrystallization at 550 °C. • The Sc,Zr-containing particle precipitation is slightly facilitated by cold rolling. • The Mn-containing particle precipitation is highly enhanced by cold rolling. • Cold rolling has no effect on activation energy of the Al{sub 3}Sc and Al{sub 6}Mn precipitation. • The texture development is affected by high solid solution strengthening by Mn.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Enhancing overall tensile and compressive response of pure Mg using nano-TiB{sub 2} particulates

A novel attempt is made to synthesize and study the isolated effects of less than two volume fraction TiB{sub 2} nanoparticulates (60 nm) on pure magnesium. New light weight Mg–TiB{sub 2} nanocomposites with superior mechanical properties compared to pure magnesium are synthesized using disintegrated melt deposition technique followed by hot extrusion. The microstructural characterization studies revealed that the samples exhibited fairly uniform distribution of TiB{sub 2} nanoparticulates with minimal porosity and good interfacial integrity between Mg matrix and TiB{sub 2} particulates. The coefficient of thermal expansion results indicates that the addition of 0.58, 0.97, and 1.98 vol.% TiB{sub 2} nanoparticulates marginally improves the dimensional stability of pure magnesium. A significant improvement in the room temperature tensile properties of pure magnesium was observed with the addition of less than two volume fraction TiB{sub 2} nanoparticulates. The synthesized Mg 1.98 vol.% TiB{sub 2} nanocomposite revealed the best room temperature tensile properties with a significant increase in the 0.2% tensile yield strength by ∼ 54%, ultimate tensile strength by ∼ 15% and fracture strain by ∼ 79% when compared to pure Mg. The X-ray diffraction studies indicated changes in the basal plane orientation of pure Mg with the addition of nano-TiB{sub 2} particulates. A maximum tensile fracture strain of ∼ 16% is achieved with the addition of 0.97 vol.% TiB{sub 2}. The room temperature compressive properties of the nanocomposites reveal that the addition of 1.98 TiB{sub 2} increases the 0.2% compressive yield strength of Mg by ∼ 47% and ultimate compressive strength by ∼ 10% with a marginal increase in the fracture strain (∼ 11%). Reduction in tensile–compression yield asymmetry was observed for Mg 0.58 and 0.97 vol.% TiB{sub 2} nanocomposites which can be attributed to the weakening of the strong basal texture of pure Mg. - Highlights: • First attempt is made to synthesize and characterize Mg-TiB{sub 2} nanocomposites. • XRD studies indicate nano TiB{sub 2} addition modifies the basal texture of pure Mg. • Maximum tensile fracture strain of ∼ 16 % in Mg 0.97 vol.% TiB{sub 2} nanocomposite. • Hardness values of Mg-TiB{sub 2} composites indicate superior tribological properties.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Structural properties of pure and Fe-doped Yb films prepared by vapor condensation

Ytterbium and iron-doped ytterbium films were prepared by vapor quenching on Kapton substrates at room temperature. Structural characterization was performed by X-ray diffraction and transmission electron microscopy. The aim was to study the microstructure of pure and iron-doped films and thereby to understand the effects induced by iron incorporation. A coexistence of face centered cubic and hexagonal close packed-like structures was observed, the cubic-type structure being the dominant contribution. There is an apparent thickness dependence of the cubic/hexagonal relative ratios in the case of pure ytterbium. Iron-clusters induce a crystalline texture effect, but do not influence the cubic/hexagonal volume fraction. A schematic model is proposed for the microstructure of un-doped and iron-doped films including the cubic- and hexagonal-like structures, as well as the iron distribution in the ytterbium matrix. - Highlights: • Pure and Fe-doped Yb films have been prepared by vapor condensation. • Coexistence of fcc- and hcp-type structures was observed. • No oxide phases have been detected. • Fe-clustering does not affect the fcc/hcp ratio, but favors a crystalline texture. • A schematic model is proposed to describe microscopically the microstructure.

36 MATERIALS SCIENCE↗
DOE OSTI2014

The microstructure and mechanical behaviors of the Ti–6.5Al–3.5Mo–1.5Zr–0.3Si alloy produced by laser melting deposition

The microstructure and mechanical properties of the Ti–6.5Al–3.5Mo–1.5Zr–0.3Si alloy produced by laser melting deposition have been investigated. The columnar grains of the Ti–6.5Al–3.5Mo–1.5Zr–0.3Si alloy due to the layer-by-layer epitaxial growth from the underlying template grains during laser melting deposition, which is roughly parallel to the deposition direction, had been found by optical microscopy; strong [101{sup ¯}2]{sub α} crystallographic texture has been confirmed by X-ray diffraction and electron backscattered diffraction. Depending on the last heating history, the microstructure of the alloy undergoes a continued change opposite to the deposition direction: martensitic α′ (transformed β); coarsened primary α laths with transformed β; coarsened primary α laths; and the fine basketweave microstructure with a few coarsened α laths or annealed martensitic α′. The average Vickers micro-hardness value of the alloy is 364 HV. The alloy parallel to the deposition direction presents lower tensile strength (925 MPa) and better elongation (18.8%), compared with 1025 MPa and 8.2% of that vertical to the deposition direction, which has been discussed using its microstructure characterization. - Highlights: • The columnar grains and strong [101{sup ¯}2]{sub α} crystallographic texture of the Ti–6.5Al–3.5Mo–1.5Zr–0.3Si alloy due to the epitaxial growth from the underlying template grains • The microstructure evolution of the alloy depends on the last heating history. • The specimen parallel to the deposition direction presents lower ultimate tensile strength and higher elongation than the specimen vertical to the deposition direction.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Microstructure evolution of 7050 Al alloy during age-forming

The microstructure evolution of the 7050 Al alloy treated by age-forming was studied using a designed device which can simulate the age-forming process. The grain shape, grain boundary misorientation and grain orientation evolution of 7050 Al alloy during age-forming have been quantitatively characterized by electron backscattering diffraction technique. The results show that age-forming produced abundant low-angle boundaries and elongated grains, which attributed to stress induced dislocation movement and grain boundary migration during the age-forming process. On the other side, the stress along rolling direction caused some unstable orientation grains to rotate towards the Brass and S orientations during the age-forming process. Hence, the intensity of the rolling texture orientation in age-formed samples is enhanced. But this effect decays gradually with increasing aging time, since stress decreases and precipitation hardening occurs during the age-forming process. - Highlights: • Quantitative analysis of grain evolution of 7050 Al alloys during age-forming • Stress induces some grain rotation of 7050 Al alloys during age-forming. • Creep leads to elongate grain of 7050 Al alloys during age-forming. • Obtains a trend on texture evolution during age-forming applied stress.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Grain size dependence of dynamic mechanical behavior of AZ31B magnesium alloy sheet under compressive shock loading

The effects of grain size on the dynamic deformation behavior of rolled AZ31B alloy at high strain rates were investigated. Rolled AZ31B alloy samples with grain sizes of 6, 18 and 37 μm, were subjected to shock loading tests using Split Hopkinson Pressure Bar at room temperature and at a strain rate of 1100 s{sup −} {sup 1}. It was found that a double-peak basal texture formed in the shock loaded samples. The strength and ductility of the alloy under the high strain-rate compressive loading increased with decreasing grain size. However, twinning fraction and strain hardening rate were found to decrease with decreasing grain size. In addition, orientation imaging microscopy showed a higher contribution of double and contraction twins in the deformation process of the coarse-grained samples. Using transmission electron microscopy, pyramidal dislocations were detected in the shock loaded sample, proving the activation of pyramidal slip system under dynamic impact loading. - Highlights: • A double-peak basal texture developed in all shock loaded samples. • Both strength and ductility increased with decreasing grain size. • Twinning fraction and strain hardening rate decreased with decreasing grain size. • ‘g.b’ analysis confirmed the presence of dislocations in shock loaded alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Dislocation density evolution of AA 7020-T6 investigated by in-situ synchrotron diffraction under tensile load

The dislocation density evolution along the loading axis of a textured AA 7020-T6 aluminum alloy during uniaxial tension was investigated by in-situ synchrotron diffraction. The highly parallel synchrotron beam at the High Energy Materials Science beamline P07 in PETRA III, DESY, offers excellent conditions to separate different influences for line broadening from which micro-strains are obtained using the modified Williamson–Hall method which is also for defect density investigations. During tensile loading the dislocation density evolution was documented from the as-received material (initial micro-strain state) to the relaxation of the strains during elastic deformation. After yield, the increasing rate of dislocation density growth was relatively fast till half-way between yield and UTS. After that, the rate started to decrease and the dislocation density fluctuated as the elongation increased due to the generation and annihilation of dislocations. When dislocation generation is dominant, the correlation between the flow stress and dislocation density satisfies the Taylor equation. Besides, a method to correct the thickness effect on peak broadening is developed in the present study. - Highlights: • In-situ synchrotron diffraction was applied to characterize peak broadening. • Dislocation evolution along the loading axis during uniaxial tension was investigated. • A method to correct the sample thickness effect on peak broadening was developed. • Dislocation density and flow stress satisfy the Taylor equation at a certain range. • The texture before load and after sample fracture was analyzed.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Strain softening during tension in cold drawn Cu–Ag alloys

Experiments were conducted on Cu–0.1wt.%Ag alloys to evaluate the influence of producing procedures and annealing conditions on microstructure evolution and mechanical properties of Cu–Ag alloys. Optical microscopy (OM), electron back-scattered diffraction (EBSD), X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used for microstructural evaluation and mechanical properties were characterized by tensile tests. The results indicated that hot-extruded Cu–Ag alloys had a typical dynamic recrystallized microstructure with equiaxed grains. Cold drawing at room temperature leaded to partial recrystallized microstructure with a mixture of coarse and fine grains. The dominate {001}<100 > cubic texture formed during hot extrusion was changed to be {112}<111 > copper texture by cold drawing. Strain softening occurred during room temperature tension of cold drawn Cu–Ag alloys with an average grain size of 13–19.7 μm. - Highlights: • Strain softening occurred during tension of Cu–Ag alloys with coarse grain size. • Work hardening was observed in hot-extruded and annealed Cu–0.1wt.%Ag alloys. • Strain softening was ascribed to dynamic recovery and dynamic recrystallization.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Monitoring micro-crack healing in an engineered cementitious composite using the environmental scanning electron microscope

Environmental Scanning Electron Microscopy (ESEM) is used to study the origin of micro-crack healing in an Engineered Cementitious Composite (ECC). ESEM images were acquired from ECC specimens cut from pre-cracked, dog-bone samples which then subjected to submerged curing followed by exposure to the natural environment. The mineralogical and chemical compositions of the healing products were determined using the EDX facility in the ESEM. It is shown that the precipitation of calcium carbonate is the main contributor to micro-crack healing at the crack mouth. The healing products initially appeared in an angular rhombohedral morphology which then underwent a discernable transformation in size, shape and surface texture, from relatively flat and smooth to irregular and rough, resembling the texture of the original surface areas surrounding the micro-cracks. It is also shown that exposure to the natural environment, involving intermittent wetting/drying cycles, promotes additional crystal growth, which indicates enhanced self-healing capability in this environment. - Highlights: •ESEM with EDX used to characterize the origin of micro-crack healing in an ECC •Evolution of healing precipitates studied at three specific locations over four weeks •Specimens exposed to laboratory environment, followed by the natural environment •Calcium carbonate is the main contributor to crack healing at the crack mouth. •Outdoor exposure involving intermittent rain promotes additional crystal growth.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Twinning behaviors of a rolled AZ31 magnesium alloy under multidirectional loading

The microstructure and texture evolution of an AZ31 magnesium rolled sheet during quasi-static compression at strain rates of 10{sup −3} s{sup −1} has been investigated by in situ electron backscattered diffraction. The influence of the initial and pre-deformed texture on the predominant deformation mechanisms during compression has been examined. It has been found that extensive grain reorientation due to (10 − 12) tensile twinning appeared when compressed along transverse direction. Tensile twin variants were observed under this loading condition, and different variants will cause an effect to the following deformation. Several twinning modes occurred with continuative loading along rolling direction. - Highlights: •Twinning behaviors were investigated through in situ multidirectional compressive tests. •Deformation behavior was affected by the twin variants. •Four types of twinning behaviors were observed during deformation process.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructural control of FeCrAl alloys using Mo and Nb additions

The effects of Mo and Nb additions on the microstructure and mechanical properties of two FeCrAl alloys were studied in this paper. Fine and uniform recrystallized grain structures (~ 20–30 μm) were achieved in both alloys through suitable annealing after warm-rolling. The formation of Fe 2 Nb-type Laves phase precipitates in the Nb-containing FeCrAl alloy effectively stabilized the deformed and recrystallized microstructures. The Mo-containing FeCrAl alloy exhibited strong γ texture fiber after annealing at 650–900 °C, whereas the annealed Nb-containing FeCrAl alloy had much weaker texture. Finally, both strength and ductility decreased as the grain size increased in both alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Multiscale mechanical behavior and microstructure evolution of extruded magnesium alloy sheets: Experimental and crystal plasticity analysis

Highlights: • Experimental stress-strain responses were reproduced by CPFE simulation based on Voronoi grains on three strain paths. • Textures predicted by simulation were in accordance with the ones measured by EBSD at the strain of 0.085. • Deformation heterogeneity in slip-dominated cases was found more significant than that in twin-favored case. • For slip-dominated cases, both high m′ value and high SFs in adjacent grains are responsible for strain localization. - Abstract: A phenomenological crystal plasticity finite element (CPFE) model based on Voronoi grains was applied to reproduce basic deformation features of a hot-extruded magnesium alloy sheet under various strain paths. Corresponding experimental investigations, including mechanical tests, electron back scattered diffraction (EBSD) measurements and optical observation, were also carried out as either a validation or a supplement of the numerical results. Predicted average stress-strain responses and texture evolution are in good accordance with measured ones. Furthermore, deformation heterogeneity at the mesoscopic and intergranular scale were investigated based on the proposed model. At the mesoscale, the heterogeneity in the slip-dominated cases tends to develop continuously, whereas the heterogeneity is retarded in twin-favored deformation. At the intergranular scale, it is concluded from the slip-dominated case that a high slip-transfer parameter and high Schmid factors (SFs) of principal slip systems in adjacent grains could accommodate higher local strain.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Coincidence site lattice boundary mechanism for the preferred growth of Goss and Cube grains during annealing in an Al-Cu-Mg alloy

Highlights: • Both Goss and Cube grains are recrystallized out of Brass matrix. • Boundary character between Brass and Goss grains was Σ9, and that between Brass and Cube was Σ5. • Σ9 and Σ5 boundaries only transitionally appeared during recrystallization. • Temperature had decisive effect on the formation and mobility of CSL boundaries. • Σ9 and Σ5 boundaries with high index planes were highly mobile. - Abstract: The formation mechanism of recrystallized textures in an Al-Cu-Mg alloy was investigated by means of three dimensional orientation distribution functions (ODFs) and in-situ electron back-scattered diffraction (EBSD). The results showed that in the hot-rolled alloy with a very sharp Brass texture but weak Copper and S orientations, both Goss and Cube grains were recrystallized out of parent Brass matrix. In-situ EBSD analysis revealed that characteristic boundary between Brass and Goss grains to be Σ9, while that between Brass and Cube grains to be Σ5. Frequency of Σ9 and Σ5 boundaries increased quickly at early stage and then reduced gradually with the process of recrystallization. Annealing at a higher temperature (320 °C) was found to be beneficial for the formation of Σ9 boundary, while at lower one (300 °C), Σ5 boundary became dominant. Besides, with temperature decreasing from 320 to 300 °C, the mobility of Σ9 boundaries was greatly degraded, but relatively, Σ5 boundaries still behaved highly mobile. Principally, the preferred growth of recrystallized Goss and Cube grains was respectively attributed to the high mobility of Σ9 and Σ5 boundaries with high index planes that the square sum of plane index was larger than 3.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure of titanium on complex deformation paths: Comparison of ECAP, KOBO and HE techniques

Highlights: • Method for producing CP titanium rods for medical implants is searched. • Three processing methods producing ultra-fine grain titanium are compared. • Microstructure and textures are examined and analysed. • Mechanical characteristics are determined based on microhardness and tensile tests. • Hydrostatic extrusion (HE) leads to the best properties of titanium rods for medical implants. - Abstract: In this work samples of commercial purity grade 2 titanium were severely deformed by three different extrusion techniques: equal-channel angular pressing (ECAP), extrusion through oscillating die (KOBO), and hydrostatic extrusion (HE). Resulting microstructures and mechanical properties of processed titanium samples are studied and compared with regard to potential application as a material for dental implants. The obtained results demonstrate the effect of different strain paths, involved by three applied deformation methods, on microstructure refinement, mechanical properties and textures of the studied material. Heterogeneous microstructures with bimodal grain size distributions are observed for all deformation techniques in the examined material, however differences in their internal structures and grain boundary distributions point to different grain refinement mechanisms. The fraction of ultra-fine grains is the highest in titanium deformed by HE. Also the internal grain fragmentation is the most important after HE deformation. This leads to the best mechanical and microstructural properties obtained in this type of deformation. Consequently, the HE process seems to be very interesting for production of material for medical implants.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Multi-scale and multi-technic microstructure analysis of a linear friction weld of the metastable-β titanium alloy Ti-5Al-2Sn-2Zr-4Mo-4Cr (Ti17) towards a new Post-Weld Heat Treatment

Highlights: • Soft joint showing sharp macro-zones and marked by asymmetrical process effects • Gradient of thermomechanical loads identified through progressive stages of transformation • Highly textured recrystallized β grains at the joint core with distorted β lattice • Lattices, phase fractions, microstructures and hardness homogenized after heat treatment - Abstract: Linear Friction Welding (LFW) is a solid-state joining process producing narrow joints mainly developed for the aircraft industry. The Thermo-Mechanical Processing (TMP) loads imposed on the material cause complex microstructure transformations. This study aimed at characterizing the local microstructures and crystallographic configurations to identify the mechanisms impacting the stability and the mechanical properties of a Ti17 LFW joint with the objective of establishing an innovative homogenizing Post-Weld Heat Treatment (PWHT). The process caused a narrow zone of ±2 mm from the friction interface to reach the isothermal α → β transformation temperature under a heating rate of 500 K/s followed by quenching (−100 K/s). The TMP resulted in the formation a ±3 mm wide soft Process Affected Zone (PAZ) delimited by three characteristic zones: the Welding Line (WL width ≈ 400 μm), The Thermo-Mechanically Affected Zone (TMAZ width ≈ 1 mm) and the Heat Affected Zone (HAZ). β TMP resulted in the total dissolution of the α phase in the joint core (WL + TMAZ) and formed strongly textured {110}<111> β recrystallized grains in the WL by continuous dynamic recrystallization of squeezed prior-β grains in the TMAZ. α + β TMP led to a gradual loss of hardness in the HAZ whose microstructure is similar to the one of the base material (BM) but is subject to gradual α laths dissolution due to the local temperatures experienced during LFW. A PWHT consisting in a β annealing followed by an α + β ageing resulted in a uniformly hardened weld with a homogenized Widmanstätten microstructure in the whole assembly.

36 MATERIALS SCIENCE↗