Laser nitriding of iron: Influence of the laser parameters on the nitriding efficiency

Laser nitriding of Armco iron in nitrogen was studied for KrF-excimer-laser irradiation. The influence of the energy density and number of pulses on the nitrogen take-up and the nitride phases formed was investigated using Resonant Nuclear Reaction Analysis (RNRA) and Mössbauer spectroscopy. Besides the original a-iron, austenite-Fe(N), martensite-Fe(N),-Fe₂₊N, and-Fe₁₆N₂ were identified. The fraction of the e-phase was found to increase with the number of pulses and the energy density. A threshold energy density of 1.8(2) J/cm² for the laser nitriding process was found.     

Radiation detected resonance ionization spectroscopy on208Tl and242fAm

An ultra-sensitive laser spectroscopic method has been developed for the hyperfine spectroscopy of short-lived isotopes far off stability produced by heavy ion induced nuclear reactions at very weak intensity (> 1/s). It is based on resonance ionization spectroscopy in a buffer gas cell with radiation detection of the ionization process (RADRIS). As a first on-line application of RADRIS optical spectroscopy at^242fAm fission isomers is in progress at the low target production rate of 10/s. The resonance ionization has been performed in two steps utilizing an excimer dye laser combination with a repetition rate of 300 Hz. The first resonant step proceeds through terms which correspond to wavelengths of 466.28, 468.17 or 426.56 nm; the second non-resonant step is achieved with the 351 nm radiation of the excimer laser itself, running with XeF. The frequency scans of the tuneable dye laser at 466.28 and 468.17 nm exhibit broad resonance ionization signals, the latter with a large isotope shift between^242fAm and²⁴³Am which is in accordance with the large quadrupole moment of the^242fAm fission isomer.Work supported by the Bundesministerium für Forschung und Technologie under contract 06 MZ 188 I.     

First observation of a resonance ionization signal on242mAm fission isomers

The feasibility of a hyperfine spectroscopy on^242mAm fission isomers has been demonstrated at the low target production rate of 10/s. The experimental method employed is based on resonance ionization spectroscopy in a buffer gas cell with detection of the ionization process by means of the fission decay of the isomers. The resonance ionization has been performed in two steps, utilizing an excimer dye laser combination with a repetition rate of 300 Hz. The first resonant step proceeds through theJ=7/2 term at 21440.35 cm⁻¹, which has been excited with the tuncable dye laser beam of a wavelength of 466.28 nm, the second non-resonant step is achieved with the 351 nm radiation of the excimer laser itself, running with XeF. The frequency scan of the tuneable dye laser exhibits a broad resonance ionization signal, the width of which is most likely explained by the magnetic hyperfine interaction.     

Laser nitriding of iron: Nitrogen profiles and phases

Armco iron samples were surface nitrided by irradiating them with pulses of an excimer laser in a nitrogen atmosphere. The resulting nitrogen depth profiles measured by Resonant Nuclear Reaction Analysis (RNRA) and the phase formation determined by Conversion Electron Mössbauer Spectroscopy (CEMS) were investigated as functions of energy density and the number of pulses. The nitrogen content of the samples was found to be independent of the number of pulses in a layer of 50 nm from the surface and to increase in depths exceeding 150 nm. The phase composition did not change with the number of pulses. The nitrogen content can be related to an enhanced nitrogen solubility based on high temperatures and high pressures due to the laser-induced plasma above the sample. With increasing pulse energy density, the phase composition changes towards phases with higher nitrogen contents. Nitrogen diffusion seems to be the limiting factor for the nitriding process.     

Isotope shift and hyperfine structure measurements at the242f Am fission isomer

Istope shift and hyperfine structure measurements have been performed for the^242fAm fission isomer with target production rates of only a few per second. The method is based on resonance ionization spectroscopy (RIS) in a buffer gas cell with radioactive decay detection of the ionization process (RADRIS). A relative isotope shift ratioX _exp=IS^242f,241/ IS^243,241=41.7±0.9 has been measured for the 500.02 nm transition corresponding to a nuclear parameter ^242f,241=5.4±0.3 fm². The analysis of the quadrupole moment based on the deformed Fermi-model of the nuclear charge distribution including second order corrections results inQ ₂₀=38.2 ±1.4( _–0.8 ^+0.4 )_model eb. The measurement of the hyperfine structure splitting of the transition at 466.28 nm yields a negativeg-factor and a nuclear spin ofI=2 orI=3.Work supported by the Bundesministerium für Bildung und Forschung under contract 06 MZ 5661.     

Characterization of laser-nitrided iron and sputtered iron nitride films

Laser-nitriding may be a promising technique for substituting conventional nitriding processes. We have irradiated pure iron with pulses of an excimer laser and achieved high nitrogen contents in a thin surface layer. We found that the nitrogen is dissolved into -Fe, leading to a large amount of retained austenite. This was also verified by X-ray diffraction (XRD) measurements. Three subspectra can be resolved in the Mössbauer spectra (CEMS) for this nitrogen austenite. The nitrogen concentration can be calculated in terms of site occupation, indicating a content as high as 16(1) at%, which is consistent with the results of Rutherford backscattering spectroscopy (RBS), resonant nuclear reaction analysis (RNRA) and Auger electron spectroscopy (AES) measurements. This is more than the solubility limit for -Fe(N). By reactive magnetron-sputtering it is possible to produce thin iron nitride films of various stoichiometries. We report on the production of-Fe _x N and FeN _y films. These films were again characterized by CEMS, RBS, RNRA (¹⁵N(p, )) and XRD. For-Fe _x N, produced in the range 2x3 with medium nitrogen flows during reactive sputtering, the Mössbauer spectra can be well resolved in terms of different iron sites, enabling an accurate calculation of the nitrogen content. For high nitrogen flows during sputtering a phase FeN _y withy>0.5 is produced. This phase is not reported in the Fe-N phase diagram.