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Concept

Annealing (materials science)

Summary

In metallurgy and materials science, annealing is a heat treatment that alters the physical and sometimes chemical properties of a material to increase its ductility and reduce its hardness, making it more workable. It involves heating a material above its recrystallization temperature, maintaining a suitable temperature for an appropriate amount of time and then cooling. In annealing, atoms migrate in the crystal lattice and the number of dislocations decreases, leading to a change in ductility and hardness. As the material cools it recrystallizes. For many alloys, including carbon steel, the crystal grain size and phase composition, which ultimately determine the material properties, are dependent on the heating rate and cooling rate. Hot working or cold working after the annealing process alters the metal structure, so further heat treatments may be used to achieve the properties required. With knowledge of the composition and phase diagram, heat treatment can be used to adjust

Official source

https://en.wikipedia.org/wiki/Annealing_(materials_science)

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Studies on the Effect of Strain on the Electronic Properties of Ultra Thin Films of Superconducting Cuprates

Nathaniel Wooding

High Tc superconductivity in cuprates is still an unresolved topic, and one particular challenge is why in-plane compressive strain enhances Tc in ultra thin LSCO-214 films (< 40nm), whilst tensile strain diminishes it. Especially intriguing is whether altering this strain at a given doping has an effect on T* (pseudogap) or Tc (condensation/phase coherence). As the ratio between T* and Tc is so high, we systematically grew a series of BSCCO-2201 films by in house pulsed laser deposition (PLD), and then thoroughly analysed these films with X-Rays, four point resistivity measurements and XPS. We succeeded to induce strain into the films; however, the strain was lost in the annealing process necessary for superconductivity. Subsequently, we focused on LSCO-214 films, and grew a series of strained ultra thin films of this compound. While the films were superconducting, none of our samples showed enhanced superconduc- tivity, probably due to growth disorder.Therefore, we eventually studied high quality films grown by MBE from BNL. We used the low energy muon beamline at PSI to perform μSR studies on two different com- pressive strain states. The successful measurements of the penetration depth and Ginzburg- Landau parameter κ on ultra thin films of this type using low energy muons showed the benefits of this technique. As the 2 films were of different thicknesses, further studies need to be done to disentangle which observed effects are due to strain and/or variation in c-axis, and which are due solely to thickness. Our accumulated results and those of other groups, (notably Naito et. al. at NTT) on strain in LSCO-214 films, and the ensemble of data, including our study, indicate that most likely it is a phase coherence enhancement due to the in-plane compressive strain that raises the Tc. In summary, in addition to the succesful implementation of PLD heteroepitaxy, XRD analysis and ρ(T) studies of LSCO-214 films we were able to establish that: 1. Phase coherence is improved by in plane compressive strain, hence Tc enhancement 2. Tc also seems to scale with apical oxygen, as previously reported by H. Keller et. al., and local distortions around the copper-oxygen tetrahedra 3. Last but not least, we were even able to induce strain into BSCCO-2201 films, yet at present the full electronic properties of this system are neither measured nor under- stood. Finally, further systematic studies on μSR are proposed, and are indeed underway at PSI, to further elucidate the microscopic role of strain in the mechanism of high Tc superconductivity.

EPFL2013

The formation and growth of cracks by irradiation assisted stress corrosion cracking (IASCC) in light water reactor internals is a critical issue for a safe long-term operation of nuclear power plants. The IASCC susceptibility at relatively low dose is dominated by conventional mechanisms such as radiation-induced segregation and radiation hardening. However, the ageing of the nuclear fleet combined with the increase of their life-span reveals other mechanisms that could play an important role on IASCC susceptibility. Recent studies show that a huge amount of helium (He) can be accumulated in reactor internal components of pressurized water reactors (PWR) after long-term operation. This occurrence could significantly increase the IASCC susceptibility at high doses. The main objective was to investigate the He effects on IASCC susceptibility of the solution-annealed (SA) and 20% cold-worked (CW) austenitic steel 316L. SA and CW miniaturized tensile samples and a SA plate were homogeneously implanted up to 1000 appm He. He was implanted at ~45 MeV and 300°C at the cyclotron in CEMHTI/CNRS (France). Slow strain rate tests (SSRT) in air and in high-temperature water were then carried out on SA, CW, post-implantation annealed (PIA) and as-implanted samples; instrumented nanoindentation tests were performed at room temperature on non-implanted and implanted specimens; and scanning electron microscope and transmission electron microscope were employed for fractography and microstructural characterization. The results of SSRTs in high-temperature air and in hydrogenated high-temperature water showed that homogenized implanted He up to 1000 appm corresponding to a displacement damage of about 0.16 dpa (displacement per atom) does not produce intergranular cracking and IASCC. However, the deformation microstructure of non-implanted SA/CW is characterized by high dislocation density arranged in cell walls separated by relatively dislocation-free regions, while the as-implanted SA samples (> 0.05 dpa) exhibit a more planar deformation microstructure. Characterization of as-implanted CW and PIA samples did not show any significant implantation effect on the deformation microstructure. PIA of the He implanted plate was carried out from 650 to 1000°C for 1h to increase the helium grain boundary coverage, and to reproduce the observed microstructure of the replaced reactor internal components that showed IASCC and use the results for the PIA of tensile samples. The transmission electron microscope investigations showed that an increase of the annealing temperature causes an average bubble size increase and density decrease. The average He bubble size and distribution in the grain interior and on the grain boundary were similar in the range of temperatures studied. In both cases, bubbles grew by the Ostwald ripening mechanism. No preferential He build-up took place on the grain boundaries. The increase of yield stress produced by He bubbles was calculated with three distinct dislocation-localized obstacle and compared to the tensile test results. The bubble strength estimated for these models was used to assess their validity and to compare the results to published data. Finally, nano-indentation tests in SA, CW, as-implanted SA and PIA (650 to 850°C for 1h) samples did not show He effects on grain boundaries strength. However, the average hardness of the grain interior increased with the He implantation and decreased increasing the PIA temperature.

EPFL2018

An Experimental Setup for Heterogeneous Catalysis on Atomically Defined Metal Nanostructures

Jean-Guillaume De Groot

The main objective of this PhD thesis is to link the atomic scale structure to the catalytic properties of self-assembled nanostructures. The growth and characterization of these nanostructures was carried out in an ultra-high vacuum (UHV) chamber initially designed for the study of the kinetics of epitaxial growth of thin films and nanostructures by variable temperature scanning tunneling microscopy. During this PhD thesis, we built a very sensitive and selective gas detector based on a quadrupole mass spectrometer and adapted to the geometry of this UHV system. The proper functioning of the gas detector is confirmed by temperature programmed desorptions of Xe on Ag(100) which demonstrate the very high sensitivity of the device of about

10^{-6}

~monolayer (ML). The zero-order desorption parameters obtained for the first monolayer of Xe adsorbed on Ag(100) are

E_d=0.22-0.23

~eV with a prefactor

\nu_0

between

4\times10^{12}

^{-1}

and

1 \times10^{13}

^{-1}

. An exchange process between Fe adatoms and Ag atoms from the Ag(100) surface is identified by means of temperature programmed desorption of N

_2

. Desorption spectra suggest that the exchange is complete from an annealing temperature of 140~K. Our study of the catalytic activity of metal nanostructures focuses on the ability of passivated Fe clusters to adsorb N

_2

molecules without dissociating them, which is a fundamental step in the bio-inspired heterogeneous catalysis of ammonia. The first system investigated for the growth of Fe clusters is MgO/Ag(100). Diffusion of Fe adatoms deposited on a MgO monolayer is observed from an annealing temperature of 280~K onwards. Fe clusters with an average size of

12.1\pm 0.5

~atoms are obtained on a MgO monolayer by thermal ripening of 0.072~ML of Fe deposited at 40~K. No sign of N

_2

adsorption was observed on these clusters by thermal programmed desorption investigation. The second system chosen for the growth of Fe clusters is graphene/Ir(111) obtained by chemical vapor deposition. The deposition of 0.3 and 0.4 ML of Fe on a graphene/Ir(111) sample at 50~K, followed by annealing at 300~K, generates a superlattice of Fe clusters which matches the periodicity of the moiré formed by graphene/Ir(111). The theoretically expected mean cluster size is 26 atoms for 0.3~ML of Fe, and 35 atoms for 0.4~ML of Fe. The temperature stability of the clusters obtained with 0.4~ML Fe is investigated from 300~K to 600~K. It is established that Smoluchowski ripening takes place as the annealing temperature increases and the superlattice structure has completely disappeared after annealing at 600~K. Temperature programmed desorption of molecularly adsorbed N

_2

at 50~K on a sample with 0.4~ML of Fe deposited on graphene/Ir(111) reveals 3 desorption peaks at 120~K, 92~K, and 60~K. In addition, slow dissociation of nitrogen molecules at 50~K adsorbed on the higher energy adsorption sites is demonstrated.

EPFL2021