Degradation of elastomer by heat and/or radiation

This article studied various problems on the degradation of elastomers by heat and/or radiation. Three kinds of elastomers were irradiated and evaluated by the radiation resistant property using the measurement of tensile test. The fluorine containing elastomer, which has excellent heat resistant properties, was found to be less durable for irradiation than ethylene-propylene-diene (EPDM) elastomer. Ten kinds of different compounding formulas of EPDM were prepared to investigate whether the compounding for heat resistant has durability for irradiation. The thermal exposure was performed in an air oven. The duration of thermal exposure at 140 °C was 384 h. The irradiation condition was 5.0 kGy/h at 70 °C, and the total dose was 0.9 MGy. Elongation retained was taken for the evaluation of the stability. It was found that the formulas for improving the thermal stability did not bring radiation resistant of samples in the experiment.The rate constant of the increase in CO concentration by heat and radiation was measured and defined as k_c(h) and k_c(r), respectively. The rate constant of that under the combined addition of the heat and the radiation is expressed as k_c(h + r). Eq. (1) was obtained by the experiment and it was found that there is a synergistic relationship between heat and radiation on the increase in CO concentration

(1)     

The effects of tungsten addition on the microstructural stability of 9Cr–Mo Steels

The effects of tungsten addition on the microstructure and high-temperature tensile strength of 9Cr–Mo steels have been investigated by using three different steels: M10 (9Cr–1Mo), W18 (9Cr–0.5Mo–1.8W), and W27 (9Cr–0.1Mo–2.7W) steels. The tungsten-added 9Cr steels have revealed better high-temperature tensile strength. Microchemical analysis for (Cr,Fe)₂ (C,N) revealed that the tungsten addition increased the Cr/Fe ratio, which resulted in the lattice expansion of (Cr,Fe)₂ (C,N), and then the enhanced pinning effect on the glide of dislocation. In addition, in M10 steel, the M₂₃C₆ carbides quickly grew and agglomerated, while the tungsten-added 9Cr steels revealed a fine and uniform distribution of M₂₃C₆ carbides. Dislocation recovery during tempering treatments was delayed in tungsten-added 9Cr steels, which was correlated with the stabilized precipitates and the decreased self-diffusivity of iron. It is, thus, believed that the excellent high-temperature tensile strength of tungsten-added 9Cr steels is attributed to the stabilized M₂X carbo-nitrides and M₂₃C₆ carbides and the decreased self-diffusivity of iron.     

M2N nitride phases of 9% chromium steels for nuclear applications

M₂N nitride phases of 9% chromium steels with an extra-low carbon content have been investigated using a transmission electron microscope and an energy-dispersive X-ray (EDX) spectroscopy. The steel samples were normalized for 1 h at 1050 °C and then tempered at 600-780 °C for 30 min to 5 h followed by an air cooling. Through the analyses of the electron micro-diffraction patterns and EDX data for the precipitate particles on the extracted carbon replica, two types of Cr-rich M₂N nitride phases with the same hexagonal structure but totally different lattice parameters, a = 2.80 Å/c = 4.45 Å and a = 7.76 Å/c = 4.438 Å, were determined in the steels. Four types of Cr-rich M₂N phases with different lattice parameters probably existed in the steels. The M₂N phase revealed a decrease in its Cr content, an increase in its V content as the tempering temperature was increased, and no obvious change in its content for the metal fraction with an increasing tempering time.     

The effects of Co γ-ray on poly(ethylene-co-vinyl acetate)/carbon black composites

Cables used in a nuclear power plant are irradiation suppressing ones. Until now, researches on the irradiation suppressing cables have mainly been focused on insulation materials. Therefore, in this paper, the non-isothermal crystallization behaviors and degradation characteristics of ethylene vinyl acetate-carbon black (EVA-CB), used as a shielding material, were investigated by means of the Differential scanning calorimetry (DSC) and chemiluminescence analyzer (CL). The specimens were cooled after removing thermal history at 150 °C for 5 min by changing the cooling rates to 5, 7.5, 10, 15 and 20 °C/min with DSC. In addition, after maintaining a thermal equilibrium at each temperature of 25, 50, 75, 100, 125, 150 and 175 °C, their thermoluminescence was measured for 20 min with CL equipment. The ⁶⁰Co γ-ray was used for irradiation. T_c, T₀, T_∞ and t_1/2 in the DSC experiments are found to decrease gradually as radiation dose increases. Secondly, with the CL experiment, the 0.1, 0.25 and 0.5 MGy EVA-CB composites were found to show a much smaller thermoluminescence than the intact EVA-CB composites, while the 0.75 and 1 MGy EVA-CB composites were found to show a much higher thermoluminescence than ones.     

Change in magnetic properties of MgB2 thin films after irradiation by 200 MeV Au ion beam

The SHI irradiation induced effects on magnetic properties of MgB₂ thin films are reported. The films having thickness 300-400 nm, prepared by hybrid physical chemical vapor deposition (HPCVD) were irradiated by 200 MeV Au ion beam (S_e ∼ 23 keV/nm) at the fluence 1 × 10¹² ion/cm². Interestingly, increase in the transition temperature T_c from 35.1 K to 36 K resulted after irradiation. Substantial enhancement of critical current density after irradiation was also observed because of the pinning provided by the defects created due to irradiation. The change in surface morphology due to irradiation is also studied.     

Interdiffusion of polydisperse Mw distributions subsequent to proton irradiation of PS melts

Under exposure to ionizing radiation the molecular weights of polymeric matter changes via formation of crosslinks and scissions of chains. As a result the molecular weight (M_w) distribution of a polymer depends on the applied ion fluence and differs from the initial one, which in our case is of the Schulz-Zimm type. Statistical theories can be used to estimate the M_w distribution.We study M_w distributions in proton irradiated polystyrene (PS) thin films by diffusion measurements. As chains of different degrees of polymerization diffuse unequally fast diffusion depth profiles contain information about the involved M_w distribution. Both irradiation and analysis with nuclear reaction analysis (NRA) were made at the Freiburg van de Graaff accelerator.As comparison gel permeation chromatography (GPC) measurements were conducted. However, the use of GPC is limited by the minimal amount of material needed and also does not work for very short chains in our case.Here we concentrate on the M_w distributions, the measurements and the fitting procedure will be presented elsewhere.     

Neutron irradiation of sapphire for compressive strengthening. II. Physical properties changes

Irradiation of sapphire with fast neutrons (0.8-10 MeV) at a fluence of 10²²/m² increased the c-axis compressive strength and the c-plane biaxial flexure strength at 600 °C by a factor of ∼2.5. Both effects are attributed to inhibition of r-plane twin propagation by damage clusters resulting from neutron impact. The a-plane biaxial flexure strength and four-point flexure strength in the c- and m-directions decreased by 10-23% at 600 °C after neutron irradiation. Neutron irradiation had little or no effect on thermal conductivity, infrared absorption, elastic constants, hardness, and fracture toughness. A featureless electron paramagnetic resonance signal at g=2.02 was correlated with the strength increase: This signal grew in amplitude with increasing neutron irradiation, which also increased the compressive strength. Annealing conditions that reversed the strengthening also annihilated the g=2.02 signal. A signal associated with a paramagnetic center containing two Al nuclei was not correlated with strength. Ultraviolet and visible color centers also were not correlated with strength in that they could be removed by annealing at temperatures that were too low to reverse the compressive strengthening effect of neutron irradiation.     

Neutron Irradiation Effects on Superconducting Nb-Ti Wires for Fusion Reactor

A systematic study has been carried out on Nb-Ti wire of two different kinds of metallurgical structure, to examine the effects of neutron irradiation on the critical density J_c. The samples used were Nb-47.6 a/0 Ti (sample #A) and Nb-59.8a/0 Ti (sample #B), which were aged at 380°C for 0~10⁴min and irradiated to 1.3×10¹⁸n/cm² (E _n0.1 MeV). The sample temperature during the irradiation is believed to have been below 70°C. The values of J_c of both #A and #B aged up to 50 min were found to increase with irradiation. But when aged beyond 100 min, #B had its value of J_c lowered by the irradiation. The presence of Ti enriched precipitates such as α and ω phases in the samples was surmised from the behavior shown by the critical temperature T_c. The T_c of f #A and #B changed little by irradiation when aged not longer than 100 min, but with aging beyond 500 min, #B showed a decrease in its value of T_c. This decrease indicates that the Ti concentration in the matrix may have increased through radiation-induced breakup of the above-mentioned precipitates, which, in turn, would have brought about the reduction observed in J_c upon irradiation. It is concluded that superconducting Nb-Ti wire with J_c endanced by precipitation does not appear very resistant to neutron irradiation. This underlines the importance of the choice of superconducting materials to be used in fusion reactor magnets.     

Study of polypropylene/polybutene blends modified by gamma irradiation and (high melt strength polypropylene)/polybutene blends

It is well-known that polypropylene (PP) is difficult to process as a consequence of its linear structure. It is also known that grafting of long-chain branches on PP backbone using ionizing radiation is an effective approach to achieve high melt strength polypropylene (HMS PP). Chain-scission and, in minor extend, crosslinking and grafting are the predominant reaction in order to branch PP backbone. However, if multifunctional monomers are used to promote the grafting reaction, crosslinking can surpass chain scission and grafting, reducing drawability. Therefore, in an effort to enhance the processability and so the drawability, it has been found helpful to add a small amount of polybutene-1. Gamma irradiation technique was used to induce chemical changes in blends of PP and polybutene in acetylene atmosphere (crosslinker promoter) and in HMSPP/polybutene blends. The samples were irradiated with a ⁶⁰Co source with doses of 12.5 and 20 kGy in the presence of acetylene. In this work, two different methods of blends processing were compared regarding rheological and mechanical properties. Effects on the strength and elongation at the yield point and at rupture were observed by mechanical tests and showed decrease of tensile strength and increase of elongation at rupture for samples obtained by irradiation of blends. The results from rheology demonstrated an increase in melt strength and drawability of blends.     

Critical current density changes in irradiated Nb3Sn

Söll recently modeled changes in the current-carrying capacity of superconducting Nb₃Sn after irradiation. As the dose increases, the critical current density (J_c) generally increases, reaches a maximum, and decreases. The model relates the maximum J_c for different types of irradiations to the integrated damage energy (E_D) that the irradiating particles transfer to the lattice. Earlier, Söll et al. related cirtical-temperature (T_c) decreases in irradiated Nb₃Sn to E_d, which appears more reasonable since T_c is a measure of disorder (or replacements) accompanying defect production, and the final defect configuration (or displacements) are less important. The annealing temperature for the disorder (~700°C) exceeds any of the irradiation temperatures (T_IRR); therefore, T_IRR is unimportant in the T_c experiments. However, different defect structures exhibit considerably different flux pinning and the J_c model does not consider different spatial variations of the defects during production or migration and agglomeration of the defects during high-T_IRR experiments, both of which affect flux pinning. The lack of the model to take into account the physics of the damage is the subject of this paper. Arguments are presented why the defect configurations should be considered, and recently published data is presented that conflict with the conclusions of this damage-energy model.     

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.     

Effect of 200 MeV Ag ion irradiation on structural and electrical transport properties of Fe3O4 thin films

Thin films of Fe₃O₄ have been deposited on single crystal MgO(1 0 0) and Si(1 0 0) substrates using pulsed laser deposition. Films grown on MgO substrate are epitaxial with c-axis orientation whereas, films on Si substrate are highly 〈1 1 1〉 oriented. Film thicknesses are 150 nm. These films have been irradiated with 200 MeV Ag ions. We study the effect of the irradiation on structural and electrical transport properties of these films. The fluence value of irradiation has been varied in the range of 5 × 10¹⁰ ions/cm² to 1 × 10¹² ions/cm². We compare the irradiation induced modifications on various physical properties between the c-axis oriented epitaxial film and non epitaxial but 〈1 1 1〉 oriented film. The pristine film on Si substrate shows Verwey transition (T_V) close to 125 K, which is higher than generally observed in single crystals (121 K). After the irradiation with the 5 × 10¹⁰ ions/cm² fluence value, T_V shifts to 122 K, closer to the single crystal value. However, with the higher fluence (1 × 10¹² ions/cm²) irradiation, T_V again shifts to 125 K.     

The ratchetting behavior of pressurized plain pipework subjected to cyclic bending moment with the combined hardening model

A series of six tests have been conducted using carbon steel and stainless steel cylindrical specimens having mean diameter/thickness ratios in the range 8 ≤ D_m/t ≤ 28. Each cylinder is pressurized up to its calculated design pressure and is loaded with an alternative bending moment at frequencies typical of seismic events simultaneously. Ratchetting of the cylinder wall has been observed and recorded in the hoop direction. A finite element analysis with the nonlinear isotropic/kinematic (combined) hardening model has been used to evaluate ratchetting behavior of the cylinder under mentioned loading condition. Stress-strain data and material parameters have been obtained from several stabilized cycles of specimens that are subjected to symmetric strain cycles. The finite element results are compared with those obtained from experimental set-up. The results show that initial the rate of ratchetting is large and then it decreases with the increasing cycles. The FE model predicts the hoop strain ratchetting rate to be near that found experimentally in all cases that M/M_P0.2 ≤ 1. Also, M/M_y ratios for the onset of ratchetting in stainless steel specimens are less than carbon steel specimens with same D_m/t ratios.     

Precipitate phases of a ferritic/martensitic 9% Cr steel for nuclear power reactors

One of the reasons that ferritic/martenstic steels have been considered as candidate materials for nuclear power reactors is their superior creep resistance at elevated temperature. The creep rupture strength of 9% chromium steel could be improved by a fine dispersion of secondary precipitate phase. The precipitate phases in extra-low carbon 9% chromium steel with tempered conditions were investigated by transmission electron microscope and energy-dispersive X-ray analysis. The steel specimens were normalized and then tempered at different temperatures. Niobium-rich MN nitrides (Nb_0.6V_0.3Cr_0.1)N, and two kinds of vanadium nitrides, (V_0.6Nb_0.2Cr_0.2)N and (V_0.45Nb_0.45Cr_0.1)N having a f.c.c. crystal structure, were identified in the steel specimens tempered at 600-780 °C, and 750 or 780 °C respectively. Hexagonal chromium-rich M₂N precipitate phases with different lattice parameters, a = 2.80 Å/c = 4.45 Å and a = 7.76 Å/c = 4.438 Å, were determined in the tempered steel specimens. The M₂N phase showed a decrease/an increase in its chromium/vanadium content as the tempering temperature was increased. The influence of precipitates and heat treatment conditions on the high temperature properties of 9% Cr steel was discussed.     

Effect of gamma irradiation on a polymer electrolyte: Variation in crystallinity, viscosity and ion-conductivity with dose

PEO(1 − x)NH₄ClO₄(x) samples with x = 0.18 are irradiated with gamma doses varying up to 50 kGy. DSC and XRD studies indicate, in general, a decrease in crystallinity with dose. Measurement of viscosity of aqueous solutions of the irradiated samples at the same concentration, shows that there is overall chain scission on irradiation, though there is evidence of some cross-linking also at higher doses. This is corroborated by FTIR measurements. The ion-conductivity shows a strong increase for irradiation dose 35 kGy. This suggests that there is a possibility of improving polymer electrolyte properties on gamma irradiation.     

Effects of proton irradiation on electronic structure of NdFeB permanent magnets

Effects of proton irradiation on electronic structure and atomic local structure of N35EH-type NdFeB permanent magnet were investigated by soft X-ray absorption spectrometry and Mössbauer spectrometry. The local coordination environment of Fe atoms changes after proton irradiation, and the average hyperfine field H_in of the magnets decreases from 288.4 to 286.9 kOe. The effects of irradiation on Fe atoms local environment at different lattice sites are different. The near edge structure of Fe L₃ edge is changed, indicating the density of unoccupied state of Fe 3d electrons increases after proton irradiation.     

The effect of neutron irradiation on the fiber/matrix interphase of silicon carbide composites

Given the good stability of mechanical properties of silicon carbide (SiC) under neutron irradiation, the ultimate irradiation tolerance of SiC composite materials may be limited by the fiber/matrix interphase, which is critically important to the performance of these composites. This study investigates the irradiation stability of pyrolytic carbon (PyC) monolayer and PyC/SiC multilayer interphases by tensile and single fiber push-out test techniques. Neutron irradiation was performed to doses of 0.7-7.7 dpa at temperatures from 380 to 1080 °C. Both interfacial debond shear strength and interfacial friction stress apparently decrease by irradiation, although this is not so dramatic when T_irr < 1000 °C. In contrast, the interfacial shear stresses are most affected by the higher temperature irradiation (>1000 °C). Noteworthy, these irradiation effects depend on the type of interphase material, i.e., for the pyrolytic carbon or multilayer SiC variants studied. In the range of irradiation temperature and dose, the degradation in interfacial shear properties, while measurable, is not of a magnitude to degrade the mechanical performance of the composites. This was observed for both interphase types studied. In particular, the proportional limit tensile stress decreases slightly by irradiation while the tensile fracture strength undergoes very minor change.     

Measurement of transformation temperatures and specific heat capacity of tungsten added reduced activation ferritic-martensitic steel

The on-heating phase transformation temperatures up to the melting regime and the specific heat capacity of a reduced activation ferritic-martensitic steel (RAFM) with a nominal composition (wt%): 9Cr-0.09C-0.56Mn-0.23V-1W-0.063Ta-0.02N, have been measured using high temperature differential scanning calorimetry. The α-ferrite + carbides → γ-austenite transformation start and finish temperatures, namely Ac₁, and Ac₃, are found to be 1104 and 1144 K, respectively for a typical normalized and tempered microstructure. It is also observed that the martensite start (M_S) and finish (M_f) temperatures are sensitive to the austenitising conditions. Typical M_S and M_f values for the 1273 K normalized and 1033 K tempered samples are of the order 714 and 614 K, respectively. The heat capacity C_P of the RAFM steel has been measured in the temperature range 473-1273 K, for different normalized and tempered samples. In essence, it is found that the C_P of the fully martensitic microstructure is found to be lower than that of its tempered counterpart, and this difference begins to increase in an appreciable manner from about 800 K. The heat capacity of the normalized microstructure is found to vary from 480 to 500 J kg⁻¹ K⁻¹ at 500 K, where as that of the tempered steel is found to be higher by about, 150 J kg⁻¹ K⁻¹.     

Solubility of ThO2 in Gd2Zr2O7 pyrochlore: XRD, SEM and Raman spectroscopic studies

Solubility of ThO₂ in gadolinium zirconate pyrochlore, a potential host for radioactive materials, has been investigated. The phase relations in Gd_2−xTh_xZr₂O_7+x/2 (0.0 ? x ? 2.0) systems have been established under the slow-cooled conditions from 1400 °C. XRD studies reveal that the compositions corresponding to x = 0.0-0.075 are single phasic in nature and beyond x ? 0.1 the biphasic region starts. The first biphasic region comprising of pyrochlore and thoria exist from x = 0.1-0.8, and from x = 1.2 another biphasic region consisting of gadolinia stabilized zirconia (GSZ) and thoria appears which persists till x = 1.6. The end member (i.e. x = 2.0) of the series is found to be a mixture of monoclinic ZrO₂ and thoria. Interestingly, gadolinia which has wide solubility in thoria, did not show any miscibility in thoria in the presence of zirconia. Irregular grains of Gd_1.8Th_0.2Zr₂O_7.1 as shown in SEM supports its biphasic nature. Raman spectra of heavily thoria doped (x = 0.1 and 0.2) samples, indicates the presence of Zr-O₇ mode which implies the samples are highly disordered in nature.