Long-Term Changes in a Heat Exchanger Steel

The steel ASTM A213 P22 is used for superheater outlet header in power plants. During duty cycles lasting over tens of years the temperature is of the order of 545°C and the pressure 125 atm. The microscopic changes in these steels are hard to analyze under working conditions, but they are believed to be responsible for the appearance of creeps in such devices. Investigation of the microscopic modifications will help to predict future failures due to creeps, increasing the reliability and saving a lot of money.We report the investigation of such changes in ASTM A213 P22 steel in use for 30 years as a Superheater header at Haifa power station. The analysis has been carried out using Mössbauer Spectroscopy, X-ray diffraction and optical microscopy. As a result it seems that the morphology and phase change of the carbide phases M₃C/M₇C₃ and M₂₃C₆ are the most prominent changes leading to the material failures.     

Photon and Ion-Beam Induced Processes in Materials Studied by Hyperfine Interactions

Laser nitriding and laser cementation are investigated by Mössbauer spectroscopy and complementary methods. It is demonstrated how the backscattering versions of Conversion Electron and Conversion X-ray Mössbauer spectroscopy can contribute to the investigation of surface processes, like the laser-induced formation of nitrides and carbides. Additionally, the formation of semiconducting iron disilicide can be achieved by ion-beam mixing and pulsed laser irradiation of Fe/Si bilayers. The results of both processes are compared.

     

Synthesis of highly oriented TiNx coatings by free-electron laser processing of titanium in nitrogen gas

Titanium substrates were irradiated in pure nitrogen gas by means of a free-electron laser. The treatment resulted in the formation of δ-TiN_x coatings, with surface stoichiometry x≈1 and thickness of about 15 μm. Under specific experimental conditions the nitride phase had a remarkable crystallographic texture with the δ-TiN_x(200) planes parallel to the irradiated surface, and well aligned dendrites growing normal to the surface. The mechanism of the dendritic alignment and the origin of the texture correlate with the existence of a solidification front starting at the surface, which is very peculiar for laser surface treatments. This phenomenon is explained with the help of numerical simulations. PACS 61.80.Ba; 81.15.Fg; 81.65.Lp     

Ion beam induced phase transformation in Fe–Mn bilayers: a Mössbauer study

Ion‐beam mixing of Fe–Mn bilayers induced by 100 keV krypton ions in the dose range (0.1-15)×10¹⁵ ions/cm²has been studied by means of conversion electron Mössbauer spectroscopy and X‐ray diffraction. The results indicate that a dose of about 1 ×10¹⁵ Kr⁺/cm² is sufficient to induce an appreciable mixing between the two atomic species. The α-Fe(Mn)solid solution presents a maximum at this dose, while at higher doses also the ? and γFe–Mn phases are formed in an appreciable amount. Heating of irradiated samples evidences the metastable character of ? phase and favours the growth of the terminal structures γ-Fe(Mn) and α-Mn(Fe) of the Fe–Mn equilibrium phase diagram.     

Ion-beam induced changes in magnetic and microstructural properties of thin iron films

Changes in magnetic and structural properties of 60–82 nm iron films induced by heavy-ion implantation were studied using the magneto-optical Kerr effect, M?ssbauer spectroscopy, Rutherford backscattering spectroscopy, X-ray diffraction, and X-ray absorption fine structure. The influence of ion-beam parameters (ion mass, fluence) and of sample parameters (external magnetic field and stress during implantation) were investigated. The Fe films, some of them containing a thin ⁵⁷Fe marker layer for M?ssbauer spectroscopy, were deposited on Si(100) substrates, by electron-beam and effusion-cell evaporation. The films were irradiated with ²⁰Ne, ⁵⁶Fe, ⁸⁶Kr and ¹³²Xe ions at energies chosen so that the implantation profiles peaked near the middle of the Fe films. The as-deposited films were magnetically isotropic and had a high coercivity. After ion implantation, the coercivity decreased and magnetic anisotropy developed. Both changes correlated with a decrease in the internal film stress. External mechanical stress applied during the irradiation had hardly any influence on the magnetic texture, opposite to an external magnetic field applied during or before ion implantation. The results are compared with those obtained for ion-irradiated polycrystalline Ni films and epitaxial Fe films and discussed with respect to the role of radiation-induced extended defects as pinning centers.     

Laser Nitriding of Iron,Stainless Steel,and Plain Carbon Steel Investigated by Mössbauer Spectroscopy

Nitriding is a common method for improving the hardness, mechanical properties, wear and corrosion resistance of metals. Laser nitriding of metals is an efficient process, where the irradiation of surfaces in air or nitrogen atmospheres with short laser pulses leads to a fast take-up of nitrogen into the irradiated surfaces. This process has been extensively investigated for pure iron, but usually, no tools or functional parts are made of pure iron. Mainly steel or cast iron is used as a base material. Therefore, when looking for technical applicability, also the influence of alloying elements on the laser nitriding process is of great interest. Besides the pure iron various carbon steels and an austenitic stainless steel were studied in laser nitriding experiments in order to investigate the influence of the material itself. Here, the process is investigated via Conversion Electron and X-ray Mössbauer Spectroscopy (CEMS and CXMS), Resonant Nuclear Reaction Analysis (RNRA), and X-Ray Diffraction (XRD). It appears that carbon steels are even better suited for the laser nitriding process than pure iron, and the laser nitriding also works efficiently for the stainless steel which is normally difficult to be nitrided.     

Laser-produced iron nitrides seen by Mössbauer spectroscopy

Mössbauer spectroscopy is a very powerful tool to investigate technological processes performed mainly at the surface of materials. Nitriding of metals and steel is well established in surface engineering, and gas nitriding is used most frequently. Laser nitriding, i.e. the nitrogen take-up from the ambient gas upon irradiation of a steel surface with short laser pulses, is presented in its application to iron, stainless steel and plain carbon steels. It will be demonstrated how Mössbauer spectroscopy in combination with complementary methods (Rutherford backscattering spectroscopy, Resonant nuclear reaction analysis, Nanoindentation) can help to reveal basic mechanisms in these processes.     

Investigation of the Thermal Stability of Laser Nitrided Iron and Stainless Steel by Annealing Treatments

Laser nitriding has revealed to be a very promising and effective treatment to improve the technical properties, like surface hardness and corrosion-wear resistance, of iron and steels. The high nitrogen concentration, the fastness and precision of the treatment and the easy experimental setup make this technique very suitable for applications on industrial scale. Samples of pure iron and austenitic stainless steel have been irradiated with ns laser pulses in the UV radiation range and analyzed by means of Conversion Electron Mössbauer Spectroscopy (CEMS), Resonant Nuclear Reaction Analysis (RNRA), Grazing Incidence X-Ray Diffraction (GXRD) and Microhardness. Mössbauer Spectroscopy, in particular, is capable of detecting the phase composition of the nitrided layer and therefore represents an essential tool for these kind of analysis. The thermal stability of the treated samples have been investigated by subsequent annealings at increasing temperatures in vacuum and in air. For iron samples the annealing treatment at 250°C shows a rather drastic phase transformation from phase (fcc) into (Fe₄N) while a strong depletion of N has been observed for 400°C or higher, regardless of the ambient pressure (atmospheric or vacuum). On the other hand, the stainless steel shows a very good thermal stability up to 500°C, but higher temperatures induce a gradual decrease in the nitrogen concentration which seems to be a common feature for both pure iron and stainless steel. Furthermore, annealing in air leads to the formation of a thin oxide layer on the surface of the iron sample which is easily characterized by Mössbauer spectroscopy.     

Laser hydriding of crystalline and amorphous silicon

Crystalline and ion-beam-amorphized silicon samples were irradiated with a pulsed nanosecond excimer laser in a pure hydrogen atmosphere. The hydrogen concentration was determined via the ¹H(¹⁵N,)¹²C nuclear reaction. In the case of crystalline silicon, hydrogen incorporation into the sample surface was found to be well above the hydrogen solubility limit at thermodynamic equilibrium. The hydrogen depth profiles perfectly matched the damage profiles measured via Rutherford backscattering channeling spectroscopy. For the pre-amorphized silicon samples, the laser treatment resulted in epitaxial recrystallization of the amorphous top layer, but the hydrogen uptake was found to be negligible in that case. The experimental data were compared with the results of thermodynamic simulations of the laser–gas–material interaction. PACS 52.38.Mf; 61.72.Tt; 64.70.Dv     

Thin Films Made Fast and Modified Fast

Hyperfine Interactions - Thin films are playing a more and more important role for technological applications and there are many aspects of materials surface processing and thin film production,...