Mössbauer study of martensitic transformation in Xe ion-irradiated type 304 austenitic stainless steel

Foil specimens of type 304 stainless steel have been irradiated with Xe⁺ ions in the range of 100–400 keV and 1×10²⁰–1×10²¹ ions/m² to elucidate the dynamics of the ion-induced martensitic phase transformation in stainless steel. It has been clearly shown by depth selective conversion electron Mössbauer spectroscopy (DCEMS) that the ion-induced martensitic phase in type 304 stainless steel has grown from the surface to a depth dependent both on the ion energy and the fluence of the Xe⁺ ions. Especially, we observed by means of DCEMS that the extension of the martensitic phase into the interior of stainless steel has been induced with increasing ion energy. It is concluded from these results that the depth distribution of the ion-induced martensitic phase is stress-induced by the formation of the highly pressurized Xe⁺ inclusion in type 304 stainless steel.     

Positron beam studies of void swelling in ion irradiated Ti-modified stainless steel

The void swelling behavior of heavy ion irradiated D9 steel has been investigated using variable low energy positron beam. The normalized defect-sensitive S-parameter shows up a large increase in the depth region corresponding to the maximum radiation damage as a function of irradiation temperature. From the variation of S-parameter as a function of irradiation temperature, the peak swelling temperature has been deduced and the results are discussed.     

Surface transformation of AISI 304 stainless steel by high power diode laser

A high power diode laser was used in continuous mode to irradiate milled AISI 304 substrates in order to modify their surface morphology. Milling of the steel substrates was operated at different feeds, thus allowing the achievement of a broad range of starting surface texture, characterized by average roughness of ∼0.65-1.5 μm. Laser finishing was then operated on them by varying laser power and scan speed.The effectiveness of the laser finishing was evaluated by 3D surface profilometry and SEM imaging. Laser was found to modify the surface morphology of the irradiated zones and achieve high quality surface textures. Further, consistent trends of the amplitude, spacing and hybrid roughness parameters according to laser operational settings can often be found. Finally, mapping of the experimental data can lead to the definition of a first approximation tool, which can be profitably used for simulation and process control.     

Phase transformation of graphite irradiated by high-intensity pulsed ion beams

The microstructure and morphology of graphite irradiated by high-intensity pulsed ion beams (HIPIB) has been studied by varying the ion current density as 200, 350 and 1500 A/cm² with one to five shots. Phase transformation from graphite to diamond-like carbon (DLC) on the HIPIB-irradiated graphite was confirmed by Raman spectroscopy where a typical broadened asymmetric peak appeared in the wavenumber range of 1100-1700 cm⁻¹. Formation of DLC on the irradiated graphite strongly depended on the HIPIB parameters and preferably took place at the medium ion current density of 350 A/cm² up to five shots. Numerical simulation of ablation process was performed to explore the transformation mechanism of DLC from graphite irradiated by HIPIB. The calculation showed that the temperature profile in irradiated graphite at 350 A/cm² is almost identical to that at 200 A/cm², showing a deeper heat-affected zone in comparison with that of 1500 A/cm². Moreover, the ablation depth per shot is around 0.8 μm at 350 A/cm², higher than that of 0.4 μm at 200 A/cm² and much lower than that of 8.4 μm at 1500 A/cm², respectively. The experimental and numerical results indicate that a proper temperature and pressure repetitively created in the top layer of ablated graphite during HIPIB irradiation facilitates the phase transformation.     

Localized modification of magnetic properties in 304 stainless steel foil by MeV ion beams

MeV ions were implanted in 304 stainless steel foils to investigate the localized modification of the magnetic susceptibility associated with the phase transformation. The magnetic susceptibility was found to be increased by Au⁺ or Si⁺ implantation because of the localized formation of a martensitic phase. The magnetic susceptibility of ferromagnetic substrates was enhanced much more than that of non-magnetic substrates. The enhancement in the magnetic susceptibility for Au⁺-implanted samples was a factor of 4–5 greater than that for Si⁺-implanted samples.On leave from GLORY Ltd., Simoteno, Himeji, Hyogo 670, Japan     

Exploration of heterogeneous duplex grain structure in type 304 austenitic stainless steel using ultrasonic spectroscopy

Cyclic stress-strain tests at different temperatures for a given constant strain range on a single reference heat (9T2796) of Type 304 austenitic stainless steel showed many unexpected features. The metallographic investigations of the fatigued specimens showed existence of heterogeneous duplex grain structure of ASTM grain size numbers ranging from 1.6 to 3.2. Since it was not feasible economically to cut even a small portion, for the metallographic examination, of the machined and heat treated specimen ready for the test, a non-destructive technique was needed to sort out specimens according to their grain structures prior to testing. Results of using ultrasonic spectroscopy for this purpose are described in this work.     

Studies of solid surfaces with 100 keV 4He+ and H+ ion beams

Backscattering of ⁴He⁺ and H⁺ ions incident at 100 keV was used to detect foreign atoms on silicon and graphite surfaces, and also surface disorder on silicon. The ion beams were supplied by an ion-implantation accelerator. Energy spectra of the backscattered ions were measured by an electrostatic analyzer (ESA) which had 3 % energy resolution. Foreign atom sensitivity of this system, expressed as the atom density required to yield 10 counts, is 1.3 × 10¹²/cm² for gold, 9 × 10¹²/cm² for iron, and 3 × 10¹⁴/cm² for oxygen, at an ion dose of 0.8 microC per point. Use of an 8 microC dose lowers these limits an order of magnitude at the expense of greater surface damage and longer measurement time. The effective scattering yield as measured in the ESA departs somewhat from the Rutherford Z² dependence because of ion neutralization which depends on ion energy which in turn depends on the mass of the target atom. Ion channeling was used to supress scattering from silicon atoms beneath the surface which tends to obscure the peaks for light elements such as oxygen and carbon. The channeling phenomenon was also used to study surface disorder due to abrasion damage and damage done by the ion beam itself. Sputtering of metal films by the 100 keV ⁴He⁺ beam was negligible. However, iodine was removed from silicon surfaces at a detectable rate. This technique at 100 keV, in common with backscattering at higher energies, does not require UHV conditions. It can therefore be used in a simple vacuum system to analyze surfaces of technological interest which might be altered by the heating or the heavy ion bombardment which are required to remove adsorbed background gas layers in several other surface analytical techniques.     

Hydrogen damage in AISI 304 stainless steel studied by Doppler broadening

Hydrogen damage of AISI 304 stainless steel has been systemically investigated by measuring Doppler broadening of positron annihilation. Defect profiles of the S-parameter, the low-momentum annihilation fraction as a function of positron incident energy up to 30 keV (i.e. ∼1 μm depth) have been analyzed. Experimental results show that hydrogen damage between the surface and the bulk has a significant variation with depth, and strongly depends on the condition of hydrogen-charging, i.e. current density and charging time. It has been suggested that the increase in S-parameter near the surface after hydrogen-charging mainly comes from the formation of voids; however the increase in S-parameter in the bulk after hydrogen-charging mainly comes from the production of structural defects (dislocations). Defect densities induced due to hydrogen-charging in some cases (e.g. dislocation density in the bulk) are estimated based on the simple two-state trapping model.     

Tribological changes on SS304 stainless steel induced by nitrogen plasma immersion ion implantation with and without auxiliary heating

In order to achieve quite thick treated layers with reasonable thickness uniformity in SS304 steel, the plasma immersion ion implantation (PIII) process was run in high-temperature, up to 350 °C, to induce high thermal diffusion but avoid the white layer formation. In these experiments, we heated the sample-holder with a shielded resistive wire properly wound around it and subjected the SS samples to nitrogen glow discharge PIII with relatively low voltages (10 kV) in different temperatures. We also treated the SS samples by the traditional PIII method, slowly increasing the high voltage pulse intensities, until 14 kV at the end of processing, reaching temperatures of up to 350 °C. These modes of treatments were compared with respect to nitrogen implantation profiles, X-ray diffraction, tribology and mechanical properties. X-ray diffraction results indicated a much higher efficiency of auxiliary heated PIII mode compared to the ordinary PIII. Very prominent γ_N peaks were observed for the first mode, indicating large concentration of nitrogen in thick layers, confirmed by the nitrogen profiles measured by GDOS and AES. Improved mechanical and tribological properties were obtained for SS304 samples treated by the PIII with auxiliary heating, more than for ordinary PIII. Hardness was enhanced by up to 2.77 times, as seen by nanoindentation tests.     

Oxidation of AISI 304L stainless steel surface with atomic oxygen

Oxidation of stainless steel surface in oxygen atmosphere was investigated by Auger electron spectroscopy (AES) depth profiling. The samples made of AISI 304L stainless steel were exposed to highly non-equilibrium oxygen atmosphere at different temperatures between 300 and 800 K and for different periods between 5 and 600 s. The degree of dissociation of oxygen molecules was of the order of 10%. A thin oxide layer formed on the stainless steel surface consisted of the iron oxide. The thickness depended on the sample temperature. At room temperature it was 7 nm, and it remained the same up to 200 °C. With further increase of temperature, the thickness of the oxide layer increased and reached 40 nm at 450 °C. The thickness was independent of exposure time. The results were explained by two mechanisms of oxide growth. Up to 200 °C the oxidation was run by electro-migration, while at higher temperatures the thermal induced migration prevailed.     

Effect of He+ and H+ ion irradiation on polystyrene films probed by NIR photothermal deflection spectroscopy

+ and H⁺ ions. Photothermal deflection spectroscopy (PDS) technique was used to record the absorption spectrum in the wavelength range 1.20 μm to 2.0 μm. The evolution of the various overtone and combination bands occurring in this range has been related to the changes taking place in the polystyrene structure. Received: 1 September 1998 / Accepted: 20 November 1998 / Published online: 24 February 1999     

Fe Ion-induced phase transformation in 17/7 stainless steel

CEMS observation has showed the large difference in the fraction of the induced alpha phase between⁵⁶Fe ion and⁵⁷ion irradiation. In case of⁵⁷Fe ion irradiation, the projectile⁵⁷Fe probe atom observes the phase transformation which may be induced by itself. It is most probable that CEMS in⁵⁷Fe ion irradiation reflects the phase transformation due to compositional changes and alloying effects.     

Phase transformations and mechanical properties of stainless steel in the nanostructural state

The peculiar features of structurization and changes in mechanical properties are studied during equichannel-angular (ECA) pressing treatment and cold deformation (strain) through rolling of metastable austenitic steel up to a rolling rate of e = 2.1. It is shown that the ECA pressing treatment of austenitic steel resulted in enhancement of its strength characteristics and conserved its high plasticity values, exceeding by an order of magnitude, these characteristics after cold plastic strain, which is associated with the optimization of the kinetics of γ → α transformation.     

Mössbauer effect study of 316L stainless steel irradiated with 54 MeV12C6+ ions

Using Mössbauer effect (ME) and X-ray diffraction method, phase transformation in 316L stainless steel samples irradiated with 54MeV¹²C⁶⁺ has been studied. Phase transformation and the distribution of carbon in the samples have been discussed.     

In situ and tomographic observations of defect free channel formation in ion irradiated stainless steels

The effects of heavy-ion irradiation on dislocation processes in stainless steels were investigated using in situ irradiation and deformation in the transmission electron microscope as well as post mortem electron tomography to retrieve information on the three-dimensional dislocation state. Irradiation-induced defects were found to pose a strong collective barrier to dislocation motion, leading to dislocation pileups forming in grain interiors and at grain boundaries. The passage of multiple dislocations along the same slip plane removes the irradiation defects and leads to the eventual formation of a defect-free channel. These channels are composed of densely tangled dislocation networks which line the channel-matrix walls as well as residual dislocation debris in the channel interiors. The structures of the dislocation tangles were found to be similar to those encountered in later stages of deformation in unirradiated materials, with the exception that they developed earlier in the deformation process and were confined to the defect free channels. Also, defect free channels were found to widen through both source widening as well as complex cross-slip mechanisms.     

Measurement of the magnetic moment in a cold worked 304 stainless steel using HTS SQUID

The magnetic properties of stainless steel have been investigated using a radio frequency (RF) high-temperature superconductivity (HTS) SQUID (Superconducting QUantum Interference Device)-based susceptometer. The nuclear grade 304 stainless steel is nonmagnetic at a normal condition but it changes to a partially ferromagnetic state associated with martensitic transformation under a plastic deformation. The magnetic moment of the 304 stainless steels was increased with an increasing cold work rate, and decreased with an increasing annealing temperature. The change of mechanical properties such as yield strength and ultimate tensile strength (UTS) are also analyzed in terms of deformation-induced martensitic transformation.     

Investigation of defect structures in deuteron irradiated and deformed stainless steel 316 by positron annihilation

Abstract

Deuteron-irradiated and deformed stainless steel specimens were investigated by positron lifetime and Doppler broadening measurements. The evolution of the defect structures was studied as a function of the isochronal annealing temperature and for various degrees of deformation. A different behaviour was observed for deformed and irradiated stainless steel specimens. Evidence for vacancy clusters was found in the deuteron-irradiated steel. These clusters disappear after annealing around 900 K.     

Electron-spin-dependent 4He+ ion scattering on Bi surfaces

We studied low-energy (～ 1.55 keV) electron-spin-polarized ⁴He⁺ ion scattering on a Bi(111) ultrathin film epitaxially grown on a Si(111) substrate. We observed that the scattered ion intensity differed between the incident He⁺ ions with up and down spins even though Bi is a non-magnetic element. To analyze the origin of this spin-dependent ion scattering (the spin asymmetry), we investigated the detailed relationship between the spin asymmetry and the incident angle, the azimuthal angle, the scattering angle, and the incident energy. All the data indicate that the spin asymmetry originates from the scattering cross section owing to the non-central force in the He⁺–Bi atom binary collision. The non-central force is most likely attributed to the spin–orbit coupling that acts transiently on the He⁺ 1s electron spin in the binary collision.