Microstructure and its influence on mechanical properties of CLAM steel

The microstructure of China Low Activation Martensitic steel (CLAM) and its influence on mechanical properties were investigated. The tensile test showed that the strength of CLAM (HEAT 0603A) was higher than that of HEAT 0408B at room temperature, and the reverse results were obtained at elevated temperatures. The results indicated that the microstructure was composed of dispersived carbide particles and lath martensite with high dislocation density. The main precipitation phases were Cr-rich M₂₃C₆ carbides precipitated mainly along the lath boundaries and prior-austenite grain boundaries and Ta-rich MX particles precipitated mainly in the laths and lath boundaries. The finer lath was the main reason for the higher strength of HEAT 0603A compared with HEAT 0408B at room temperature; contrasted with the lower strength at high temperature. Heavier hot forging deformation degree was considered as the main possible reason for the decrease of martensite lath width in HEAT 0603A.     

Void swelling in a 9Cr ferritic/martensitic steel irradiated with energetic Ne-ions at elevated temperatures

In this work the void swelling behavior of a 9Cr ferritic/martensitic steel irradiated with energetic Ne-ions is studied. Specimens of Grade 92 steel (a 9%Cr ferritic/martensitic steel) were subjected to an irradiation of ²⁰Ne-ions (with 122 MeV) to successively increasing damage levels of 1, 5 and 10 dpa at a damage peak at 440 and 570 °C, respectively. And another specimen was irradiated at a temperature ramp condition (high flux condition) with the temperature increasing from 440 up to 630 °C during the irradiation. Cross-sectional microstructures were investigated with a transmission electron microscopy (TEM). A high concentration of cavities was observed in the peak damage region in the Grade 92 steel irradiated to 5 dpa, and higher doses. The concentration and mean size of the cavities showed a strong dependence on the dose and irradiation temperature. Enhanced growth of the cavities at the grain boundaries, especially at the grain boundary junctions, was observed. The void swelling behavior in similar 9Cr steels irradiated at different conditions are discussed by using a classic void formation theory.     

Study on the behavior of oxygen atoms in swift heavy ion irradiated CeO2 by means of synchrotron radiation X-ray photoelectron spectroscopy

To study the effects of swift heavy ion irradiation on cerium dioxide (CeO₂), CeO₂ sintered pellets were irradiated with 200 MeV Xe ions at room temperature. For irradiated and unirradiated samples, the spectra of X-ray photoelectron spectroscopy (XPS) were measured. XPS spectra for the irradiated samples show that the valence state of Ce atoms partly changes from +4 to +3. The amount of Ce³⁺ state was quantitatively obtained as a function of ion-fluence. The relative amount of oxygen atom displacements, which are accompanied by the decrease in Ce valence state, is 3-5%. This value is too large to be explained in terms of elastic interactions between CeO₂ and 200 MeV ions. The experimental result suggests the contribution of 200 MeV Xe induced electronic excitation to the displacements of oxygen atoms.     

Elevated-temperature tensile properties of irradiated 9 Cr-1 MoVNb steel

Normalized-and-tempered 9 Cr-1 MoVNb steel tensile specimens were irradiated in the Experimental Breeder Reactor-11 (EBR-11) at 390, 450, 500, and 550°C to ～2.1 and 2.5 × 10²⁶ neutrons/m² (> 0.1 MeV), which produced displacement damage levels of ～10 and 12 dpa, respectively. Tensile tests were conducted at the irradiation temperature and at room temperature. In addition to the irradiated specimens, as-heat-treated specimens and as-heat-treated specimens thermally aged at the irradiation for 5000 h were also tested.Thermal aging had no effect on the unirradiated tensile properties. Irradiation at 390°C increased the 0.2% yield stress and the ultimate tensile strength above those of the unirradiated control specimens. The ductility decreased slightly. After irradiation at 450, 500, and 550°C, the tensile properties were essentially the same as the unirradiated values. The hardening at 390°C was attributed to the dislocation and precipitate structure formed during the irradiation. The lack of hardening at 450°C and higher correlates with an absence of an irradiation-induced damage structure.     

Oxygen defects created in CeO2 irradiated with 200 MeV Au ions

CeO₂ films were irradiated with 200 MeV Au ions in order to investigate the damages created by electronic energy deposition. In the Raman spectra of the ion-irradiated films, a broad band appears at the higher frequency side of the F_2g peak of CeO₂. The band intensity increases as ion fluence increases. Furthermore, the F_2g peak becomes asymmetric with a low-frequency tail. In order to understand the origin of these spectral changes, an unirradiated CeO₂ film was annealed in vacuum at 1000 °C. By comparing the results for the irradiation and for the annealing, it is concluded that the broad band obtained for irradiated samples contains the peak observed for the annealed sample. The F_2g peak becomes asymmetric with a low-frequency tail by the irradiation as well as the annealing. Therefore, the above-mentioned changes in the Raman spectra caused by 200 MeV Au irradiation is closely related to the creation of oxygen vacancies.     

8 MeV electron irradiation effects in silicon photo-detectors

Results of investigations on the electrical properties of n⁺-p-p⁺ silicon (Si) photo-detectors irradiated with 8 MeV electrons are presented. The photo-detectors were irradiated with electrons of doses up to 100 kGy. Current-voltage (I-V) and capacitance-voltage (C-V) characteristics under dark conditions were measured as a function of dose. A significant change in the diffusion component of the saturation current is observed after irradiation, while the generation-recombination component of the saturation current remains almost unchanged. The series resistance is found to increase with increasing dose while the shunt resistance and carrier concentration decrease with dose. Optoelectronic properties, namely short circuit current I_sc, open circuit voltage V_oc under air mass zero illumination and spectral response, were measured at various doses. From the spectral responses of the devices, the minority carrier diffusion length was estimated.     

Damages induced by heavy ions in titanium silicon carbide: Effects of nuclear and electronic interactions at room temperature

Thanks to their refractoriness, carbides are sensed as fuel coating for the IVth generation of reactors. Among those studied, the Ti₃SiC₂ ternary compound can be distinguished for its noteworthy mechanical properties: the nanolamellar structure imparts to this material some softness as well as better toughness than other classical carbides such as SiC or TiC. However, under irradiation, its behaviour is still unknown. In order to understand this behaviour, specimens were irradiated with heavy ions of different energies, then characterised. The choice of energies used allowed separation of the effects of nuclear interactions from those of electronic ones.     

Influence of HIP pressure on tensile properties of a 14Cr ODS ferritic steel

An oxide dispersion strengthened ferritic steel with a nominal composition of Fe–14Cr–2W–0.3Ti–0.3Y₂O₃ (in wt.%) was consolidated by hot isostatic pressing at 1150 °C under various pressures in the range of 185–300 MPa for 3 h. The microstructure, microhardness and high temperature tensile properties of the steel were investigated. With increasing compaction pressure the density of specimens also increased, however OM and SEM observations revealed residual porosity in all tested specimens and similar ferritic microstructure with bimodal-like grains and numerous of large oxide particles, located at the grain boundaries. Mechanical testing revealed that compaction pressure has negligible influence on the hardness and tensile strength of the ODS steel, however improves the material ductility.     

Modifications in structural, cation distribution and magnetic properties of Co gamma irradiated Li-ferrite

Polycrystalline samples of Li_0.5Fe_2.5O₄ ferrite precursor were prepared by conventional standard double sintering ceramic technique and then irradiated with three different doses of ⁶⁰Co gamma rays. The crystal structure and phase orientation of the irradiated and unirradiated samples of Li_0.5Fe_2.5O₄ ferrite was done by using X-ray diffraction technique at room temperature. The lattice parameter of the studied samples increased due to the formation of Fe²⁺ ions under the ionizing effect of gamma radiation. The strain in the materials due to the irradiation was calculated from XRD data. Scanning electron microscope (SEM) studies indicate that the irradiation causes amorphization, especially at the grain boundaries. The cation distribution was calculated from XRD data analysis. By using cation distribution structural parameters such as theoretical lattice constant, ionic radii of available sites and the oxygen parameter ‘u’ have been calculated. The estimated cation distribution and other structural parameters shows strong influence of gamma rays on polycrystalline Li-ferrite. The magnetic properties of irradiated and unirradiated lithium ferrite were performed by using pulse field hysteresis loop technique at room temperature. Electrical properties such as diffusion coefficient and dielectric properties were carried out with the influence of gamma irradiation. Activation energy of diffusion process decreased after irradiation. The increase of diffusion coefficient with increasing dose rate of gamma irradiation was reinforced by the increase of Fe²⁺ ions and the displacement of metal ions from its original sites under the effect of gamma irradiation.     

Effect of Zirconium Addition to Austenitic Stainless Steels on Suppression of Radiation Induced Chromium Segregation at Grain Boundaries under Ion Irradiation

The effect of Zr addition to austenitic stainless steels on the suppression of radiation induced Cr segregation at grain boundaries under 400 keV He⁺ irradiation was studied. Type 316L stainless steel and steels with addition of 0.07, 0.21 or 0.41 mass% Zr were kept at 1,423K for 30 min, and then they were quenched into the water. Irradiation was done at 773K with the dose rate of 2.4×10^?4dpa/s. The total dose was 0.85 or 3.4dpa. After irradiation, profiles of Cr concentration across the grain boundaries were measured using an analytical electron microscope with 1 nm beam diameter. Concentration of Cr at the grain boundary is decreased by radiation induced segregation. However, it increased with the addition of Zr, and the Cr segregation is almost completely suppressed when Zr is added more than 0.21 mass%.

The effect of Zr addition on suppression of Cr segregation was analyzed focussing on the interaction between dissolved Zr atoms and point defects. The effect is based on vacancy trapping by the Zr atom, and the extent to which it suppresses Cr segregation can be empirically evaluated using a radiation induced segregation model by changing the effective vacancy migration energy.     

Light ion irradiation-induced phase transformation in the monoclinic polymorph of zirconia

Ion irradiation damage experiments were performed at ∼80 K on polycrystalline samples of monoclinic, slightly sub-stoichiometric zirconia (ZrO_1.98). Following irradiation with 150 keV Ne⁺ ions, the monoclinic phase was gradually replaced by a new phase. Transmission electron microscopy (TEM) observations in cross-sectional geometry and electron microdiffraction (μD) measurements revealed that the irradiated layer in a sample irradiated to a fluence of 5 × 10²⁰ Ne/m² is partially transformed to a higher symmetry phase of high crystallinity. This phase transformation is accompanied by reduction of the initial micron-sized, highly-twinned grain distribution, to a nano-phased grain structure. Grazing incidence X-ray diffraction (GIXRD) measurements revealed that the radiation-induced phase is a tetragonal polymorph of zirconia. This was verified by the existence of strong (1 0 1) diffraction maxima and weak (1 0 2) reflections (body-centered cell). Raman spectroscopy (RS) measurements were also performed in an attempt to corroborate GIXRD results obtained from the irradiated material. RS measurements in the confocal geometry agreed with GIXRD measurements, although RS was not as definitive as GIXRD. In addition to RS showing the existence of a band corresponding to a tetragonal structure at 262 cm⁻¹, a new mystery band appeared at 702 cm⁻¹ that increased in intensity as a function of irradiation fluence.     

Effect of He-pre-injection on dislocation loop formation and irradiation-induced segregation of Fe–12%Cr–15%Mn austenitic steel

The effect of He-injection on irradiation-induced segregation of aging treated Fe–12%Cr–15%Mn austenitic steels, which are candidate materials as the reduced radio-activation of structure material for nuclear and/or fusion reactors was investigated by using the 1250 kV high voltage electron microscope (HVEM) connected with an ion accelerator. The Fe–Mn–Cr steel has been irradiated at 573 K by three irradiation modes of single electron-beam irradiation, electron-beam irradiation after He-injection and electron/He⁺-ion dual-beam irradiation in a HVEM. Irradiation-induced segregation analyses were carried out by an energy dispersive X-ray analyzer (EDX) in a 200 kV FE-TEM with beam diameter of about 0.5 nm. Dislocation loops with strain contrast were formed during irradiation and the loop numbers density increased rapidly with irradiation dose for He-pre-injected specimens. Voids were not observed after irradiations with three irradiation modes up to 5.4 dpa at 573 K. Irradiation-induced segregations of Cr and Mn near grain boundary were observed in each irradiation condition, but the amounts of Mn segregation decreased in the cases of electron/He⁺-ion dual-beam irradiation compared with single electron-beam and electron-beam irradiation after He-injection conditions.     

Irradiation damage in proton irradiated palladium-iron solid solutions

Transmission electron microscopy was used to investigate the irradiation damage, in particular irradiation induced precipitation (IIP), in Pd-base alloys containing 2, 8, 12 and 18 at % Fe. The specimens were irradiated mainly using 400 keV protons at a current density of 0.16 μA/mm² over the temperature range 110 to 750°C. A few samples containing 2 and 8% Fe were also irradiated using 3 MeV NiP⁺ ions. The irradiation microstructure of the proton irradiated alloys consists of dislocation loops over the temperature range 110 to 550°C and voids up to 650°C in all the alloys. IIP of Pd₃Fe was observed only in the Pd-18% Fe alloy between 110 and 500°C, irradiated to a dose of 0.9 dpa. Pd₃Fe was associated with dislocation loops, voids and grain boundaries. IIP was not observed in the Pd-2,8 and 12% Fe alloys proton irradiated to the same dose, nor to a higher dose of 1.5 dpa. It was also not observed in the 2 and 8% Fe alloys irradiated at 600 and 700°C by 3 MeV Ni⁺ ions.The absence of IIP in the more dilute alloys is attributed to the fast back diffusion of Fe atoms, which is due to the high mobility of vacancies in these alloys. This causes the Fe concentration at the sinks to remain below the solubility limit. Therefore, even though Fe is an undersized solute, the size effect alone is not sufficient for the production of IIP at point defect sinks in most Pd-Fe alloys. It is proposed that IIP can occur only when the alloy concentration is high enough to minimize the rate of back diffusion, which depends not only on the vacancy mobility but also on the concentration gradient near point defect sinks.     

Radiation-damage in molybdenum-rhenium alloys for space reactor applications

Various Mo-Re alloys are attractive candidates for use as fuel cladding and core structural materials in spacecraft reactor applications. Molybdenum alloys with rhenium contents of 41-47.5% (wt%), in particular, have good creep resistance and ductility in both base metal and weldments. However, irradiation-induced changes such as transmutation and radiation-induced segregation could lead to precipitation and, ultimately, radiation-induced embrittlement. The objective of this work is to evaluate the performance of Mo-41Re and Mo-47.5Re after irradiation at space reactor relevant temperatures. Tensile specimens of Mo-41Re and Mo-47.5Re alloys were irradiated to ∼0.7 displacements per atom (dpa) at 1073, 1223, and 1373 K and ∼1.4 dpa at 1073 K in the High Flux Isotope Reactor at Oak Ridge National Laboratory. Following irradiation, the specimens were strained to failure at a rate of 1 × 10⁻³ s⁻¹ in vacuum at the irradiation temperature. In addition, unirradiated specimens and specimens aged for 1100 h at each irradiation temperature were also tested. Fracture mode of the tensile specimens was determined. The tensile tests and fractography showed severe embrittlement and IG failure with increasing temperatures above 1100 K, even at the lowest fluence. This high temperature embrittlement is likely the result of irradiation-induced changes such as transmutation and radiation-induced segregation. These factors could lead to precipitation and, ultimately, radiation-induced embrittlement. The objective of this work is to examine the irradiation-induced degradation for these Mo-Re alloys under neutron irradiation.     

硅对低活化马氏体钢电子辐照行为的影响

利用超高压透射电子显微镜研究了两种成分的低活化马氏体钢(CLAM钢)的辐照损伤行为。结果表明：电子辐照能在未添加硅的CLAM钢中产生辐照空洞;在450℃下辐照至14dpa时,空洞数密度约为8.7×10²¹m^－3,辐照肿胀率约为0.26％;在450℃下的辐照肿胀率明显比500℃下的高;当损伤率为2×10^－3dpa/s时,添加合金元素硅能显著提高CLAM钢的抗辐照肿胀能力,未在添加硅的CLAM钢中实验观察到辐照空洞的形成。在450℃下进行辐照时,添加硅的CLAM钢出现明显的辐照共格析出现象。     

Evidence of nanostructure formation in Ge oxide by crystallization induced by swift heavy ion irradiation

Ge oxide films were irradiated with 150 MeV Ag ions at fluences varying between 10¹² and 10¹⁴ ions/cm². The irradiation-induced changes were monitored by FT-IR spectroscopy, atomic force microscopy, X-ray diffraction and photoluminescence spectroscopy. The FT-IR spectra indicate stoichiometric changes and an increase in Ge content on irradiation. X-ray diffraction shows a crystallization of the irradiated films and presence of both Ge and GeO₂ phases. The Ge nanocrystal size, as calculated from Scherrer’s formula, was around 30 nm. The morphological changes, observed in atomic force microscopy, also indicate formation of nanostructures upon ion irradiation and a uniform growth is observed for a fluence of 1 × 10¹⁴ ions/cm².     

Helium-implanted CLAM steel and evolutionary behavior of defects investigated by positron-annihilation spectroscopy

China Low Activation Martensitic (CLAM) steel has been chosen as the primary candidate structural material for the first wall/blanket for fusion reactor. The excessive helium irradiation induced damage of CLAM steel at high temperatures and the evolution of defects were investigated in this paper. The samples were homogeneously implanted with 1e + 17 ions/cm² and 100 keV of helium at room temperature, 473, 673, and 873 K. Irradiation induced damage of CLAM steel and the annealing behavior of defects were probed by slow positron beam Doppler broadening technique. Helium implantation produced a large number of vacancy-type defects which bound with helium and formed helium–vacancy complexes. Target atoms’ displacement capacity was strengthened with rising irradiation temperatures, so the S parameter increased with increasing irradiation temperatures, and helium–vacancy complexes were main defects after helium implantation at damage layers. Helium bubbles would be unstable and the desorption of helium bubbles would promote the density of defects above 673 K. By analyzing the curves of S–W and annealing tests of irradiated specimen, it suggested that there werenot only one type of defect in damage layers. Though helium–vacancy complexes were primary defects after helium implanted, introducing excessive helium might also generated other point defects or dislocation loops in the material.     

Crack Initiation Mechanism in Non-ductile Cracking of Irradiated 304L Stainless Steels under BWR Water Environment

The deformation behavior and initiation mechanisms of intergranular (IG) and transgranular (TG) cracks in irradiated 304L stainless steel were studied by slow-strain-rate tensile tests in inert gas and simulated BWR water environments, followed by fractographic and microstructural examinations. Neutron irradiation was made in test reactors to fluences of up to 6.2x10²⁰ n/cm² (E>1 MeV). Intergranular cracking occurred in water above a critical neutron fluence of around 1 × 10²⁰ n/cm², based on the results of the SSRT tests and SEM fractography. That critical fluence is mechanistically supported by irradiated, deformed microstructures exhibiting dislocation channeling at that fluence, while radiation-induced Cr depletion at the grain boundaries was minor. Transgranular cracking of the irradiated material occurred in water below the critical fluence, initiating in the non-uniformly strained surface region of the test bar in the later stages of plastic deformation. The initiation of TG cracking is hypothesized to be related to a high density of deformation twins. Intergranular cracking is proposed to have initiated where localized slip bands terminated at grain boundaries, while TG cracking is inferred to have initiated at deformation twin boundaries. High stress and strain concentrations at grain/twin boundaries would be the common cause of non-ductile crack initiation.     

Elevated-temperature tensile properties of irradiated 214 Cr-1 Mo steel

The effect of neutron irradiation on the tensile properties of normalized-and-tempered $\text{2}\text{1}\text{4}$ Cr-1 Mo steel was determined for specimens irradiated in Experimental Breeder Reactor II (EBR-II) at 390 to 550°C. Two types of unirradiated control specimens were tested: as-heat-treated specimens and as-heat-treated specimens aged for 5000 h at the irradiation temperatures. Irradiation to approximately 9 dpa at 390° C increased the strength and decreased the ductility compared to the control specimens. Softening occurred in samples irradiated and tested at temperatures of 450, 500, and 550 °C; the amount of softening increased with increasing temperature. The tensile results were explained in terms of the displacement damage caused by the irradiation and changes in carbide precipitates that occur during elevated-temperature exposure.     

Heavy ion beam induced phenomena in polytetrafluoroethylene

This paper describes the results on thermal and chemical analysis of polytetrafluoroethylene (PTFE) film stack after high-energy heavy ion beam irradiation under atmospheric fields at room temperature. After high-energy C⁶⁺ ion beam irradiation, the PTFE film stack was separated one by one, and then the various measurements such as differential scanning calorimetric (DSC) analysis and solid-state ¹⁹F magic-angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy were performed to get information of the chemical reaction and structural change at the localized positions. By ion beam irradiation for PTFE at room temperature, it is suggested that the abnormal phenomena due to the change of morphology could be observed by DSC analysis. In the solid-state ¹⁹F-MAS-NMR spectroscopy of ion irradiated PTFE film including Bragg peak region, several new signals were observed besides the intense peak of -CF₂- at −124 ppm. The detected new signals in ion irradiated PTFE should be due to the changed chemical structures. The signals, which are assigned, to the tertiary carbon group with branching site (Y-type crosslinking site), perfluoro-propylene site and chain end methyl site were directly detected, though it was under the oxidation condition. Thus, although it was under the oxidation condition, the branching or crosslinking reaction was taken place with the chain scission in the matrix. Moreover, the branched chain length would become short, compared with EB-crosslinked PTFE. Hence, it could be suggested that the irradiation of heavy ion beam induced large amounts of intermediate species, compared with EB or γ-ray irradiation, and then, those would be reacted with each other in the localized area. Especially, in region of the Bragg peak, the ion beam induced more large amounts of intermediate species than in the other region.