The Behaviour of Hydrogen Atoms Implanted Into Metals

Accumulation of the nuclear reaction product He in fusion and fission reactor components leads to severe problems. During investigation of these problems, microanalysis of He in solids has special importance. The present paper will give a review of analytical methods, especially those based on interactions of energetic charged particles. Some of these are based on elastic scattering (proton elastic scattering, elastic recoil detection, scattering combined with coincidental detection of both scattered and recoiled ions), while others are related to nuclear reactions (i.e., 3 He(d, p) 4 He). Some other methods will also be presented (i.e., thermal desorption spectroscopy, VUV absorption spectroscopy, electron energy loss spectroscopy). Special attention will be paid to the progress made during the last 10 years.

Microanalysis of He using charged particle accelerators

We have used 20Ne and 40Ar beams with energies between 3 and 8 MeV for elastic recoil detection (ERD) analysis of hydrogen isotopes in polymer samples and have also studied the depth resolution and the radiation damage. For the investigation of polymer mixtures it was possible to improve the depth resolution of ERD down to 8 nm FWHM with-out changing the experimental setup of conventional ERD, due to the higher energy loss factor of heavier ions and a reduced stopper foil thickness. For an improved surface depth resolution heavier ions are suitable, whereas lighter elements have a larger profiling depth. We found a 20Ne beam with an energy between 4 and 6 MeV to have a maximum analysing depth of 380 nm with a near surface depth resolution of 9 nm; however, for high resolution 40Ar-ERD measurements this maximum profiling depth is reduced to 90 nm. Due to the larger Rutherford scattering cross-section of heavier ions the measuring time decreases with increasing ion mass. We have investigated the ion beam radiation damage in polymer samples and introduced beam current density limits related to polystyrene samples. These results are supported by model calculations which give approximated values of the radiation damage.

Deuterium depth profiling in polymers using heavy ion elastic recoil detection

We describe a new setup for elastic recoil detection analysis (ERDA) using our recently developed particle identification method. Before the ions and elastic recoil atoms from the target reach a silicon surface barrier detector for energy analysis, they penetrate a set of thin foils (e.g. carbon). The ion induced electron emission yield from the foils depends on the nuclear charge of the penetrating ion and it is roughly proportional to the energy loss in the foil. The emitted electrons are accelerated towards a microchannel plate (MCP), which gives a signal amplitude proportional to the number of emitted electrons. This signal is measured in coincidence with the energy signal from the surface barrier detector using our dual-parameter multichannel analyzer system M2D. Since the energy resolution is not measurably deteriorated by the particle identification our setup offers optimum depth resolution for light elements. Due to the compact design large solid angles for high sensitivity can be achieved. A new measuring chamber has been built which offers considerable improvements. The ERDA scattering angle (30° or 45°) and the target orientation can be selected for optimum depth resolution or sensitivity. Element separation for light elements has been enhanced by several improvements: A new geometry of the foil setup improves the collection efficiency for ion induced electrons onto the MCP, coating of the carbon foils with insulators enhances the electron emission yield. Finally, a new data evaluation procedure has been developed in which the pulse height spectrum of the MCP is considered to be a linear combination of individual spectra from the incident ion and of the recoil atoms. The normalized shapes of these spectra are taken from calibration measurements, the intensities are then calculated using a linear fitting algorithm and finally give the depth profiles of the elements in the target. For hydrogen in near surface layers even isotopic separation is possible. Examples for 1H and 2H in a Be matrix will be given.

A new setup for elastic recoil analysis using ion induced electron emission for particle identification

Hydrogen and helium behavior in Ti, Zr and Nb membranes of several μm thickness was investigated by Elastic Recoil Detection Analysis (ERDA) using 6 MeV O and 12 MeV C beams in the transmission geometry. The concentration depth profiles of H and He during the 4 He implantation were simultaneously measured in the membranes containing uniformly distributed H of about 0.1 at.%. During the 4 He implantation into Ti, Zr and Nb membranes, an enrichment of the H concentration was observed at the depth corresponding to the range of the implanted 4 He ions. In the Nb membrane, a reversible change of the H profile was observed on heating and cooling runs. The trapping energy of H in defects created by 10 keV 4 He implantation in the Nb membrane was estimated to be 0.14 ± 0.03 eV from the change in H concentration on cooling after the 4 He implantation at 500 K.

Application of ERDA method to study hydrogen and helium in Ti, Zr and Nb membranes

An 8 MeV 16O beam was used to profile the depth concentration of 1,2H and 4He implanted into silicon wafers and stainless steel (SUS316). The measured energy spectra of recoiled particles have been unfolded to obtain depth profiles. The TRIM'86 data have been utilized to calculate the response matrix which takes account of the energy loss of particles in the sample and absorber foil. The unfolded depth profiles have been compared with profiles estimated from the condition of sample preparation. We have adjusted the experimental conditions such as the incident and detection angles to optimize the depth resolution. The depth resolution (FWHM) is typically 35 nm for hydrogen in silicon wafers at a depth of 50 nm, and 20 nm for helium in stainless steel over the depth interval 0–150 nm, respectively. In this article we will present results of experiments and unfolding calculations.

ERDA of hydrogen and helium using an 8 MeV 16O beam

Correlation between hydrogen and helium retentions in stainless steel irradiated with helium and hydrogen

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ERDA of hydrogen and helium using an 8 MeV 16O beam

Correlation between hydrogen and helium retentions in stainless steel irradiated with helium and hydrogen