High sensitivity analysis and profiling of oxygen and nitrogen by A (d, pγ)-coincidence technique

doi:10.1016/0168-583X(90)90516-W

Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms

Volume 51, Issue 2, August 1990, Pages 152-162

https://doi.org/10.1016/0168-583X(90)90516-W Get rights and content

Abstract

For the analysis of oxygen and nitrogen in heavy matrices, (d, p) and (d, α) reactions with deuteron energies around 1 MeV are commonly employed because of their reasonable cross sections and favourable Q-values. Unfortunately, depth profiling of oxygen or nitrogen in the presence of other light elements by means of these reactions is often severely hampered due to overlapping particle groups. In the case of nitrogen, the analysis is furthermore complicated by interference between its own proton groups. However, by detecting a particular particle group in coincidence with its accompanying gamma ray transition, background particles can be suppressed by at least two orders of magnitude. By this method it is possible to determine depth profiles of oxygen or nitrogen in relatively pure samples at the ppm level or, with reduced sensitivity, in samples with severe background problems. The applicability of this technique is demonstrated in case of the reactions ¹⁶O(d, p₁)¹⁷O and ¹⁴N(d, p₅)¹⁵N for a number of oxygen- and nitrogen-containing samples. Various aspects of the experimental setup are discussed.

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Cited by (18)

Measurement of deuteron induced gamma-ray emission cross sections on nitrogen for analytical applications
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In the Nuclear Reaction Analysis (NRA) technique, the 14N(d,p)15N and 14N(d,α)12C reactions have been commonly used for nitrogen analysis due to their relatively high differential cross sections and positive Q-values [2–5]. However in these measurements, the particle spectrum becomes more complicated by interference between proton groups from deuteron-induced reactions with nitrogen as well as proton groups originating from deuteron-induced reactions on elements like oxygen and carbon which usually co-exist in the sample matrix or appear as surface contaminants [6–8]. Particle-Induced Gamma-ray Emission (PIGE) spectrometry is another favored ion-induced nuclear reaction analysis for the quantitative analysis of light elements.
Deuteron induced gamma-ray emission cross-section values from the ¹⁴N(d,pγ_4-1)¹⁵N (E_γ = 1885 keV), ¹⁴N(d,pγ_6-1)¹⁵N (E_γ = 2297 keV), ¹⁴N(d,pγ_5-0)¹⁵N (E_γ = 7299 keV) and ¹⁴N(d,pγ_7-0)¹⁵N (E_γ = 8310 keV) nuclear reactions were measured in the 600–2000 keV range of the incident deuteron energies, in 30 keV steps at the laboratory angle of 90°, utilizing a thin C₃H₆N₆ target evaporated onto a self-supporting Ag film. The thick target gamma-ray yields were measured in the same experimental setup using a thick TiN target. These measurements were conducted using the deuteron beam of the 3 MV Van de Graaff electrostatic accelerator of Nuclear Science and Technology Research Institute (NSTRI) in Tehran. The obtained results were compared with the previously reported data. The validity of the measured differential cross sections was verified through a thick target benchmarking experiment. The overall systematic uncertainty of the measured values was estimated and reported.
Application of PIGE, BS and NRA techniques to oxygen profiling in steel joints using deuteron beam
2015, Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms
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The advantage and limitation of oxygen analysis using charged particle bombardment was summarized in Cohen et al. [3]. Several papers deal with the measurement of oxygen depth profiles in different materials (see e.g. [4]), however only a few applications of IBA techniques to the investigation of steel surface using particle detection were found in literature [5–7]. The analysed depth varied between 1 and 5 μm in these applications and the energy of deuteron beam was low, 665 keV in Refs. [5,6] and 1200 keV in Ref. [7], respectively.
In order to study the oxygen content and to characterize the oxygen depth profile on the surface of welded steel joints in the function of the applied shielding gases, particle induced gamma-ray emission (PIGE), backscattering spectrometry (BS) and nuclear reaction analysis (NRA) methods were used. The measurements were carried out at 1.0, 1.4 and 1.8 MeV deuteron energies. From the PIGE oxygen and carbon elemental maps (1000 × 1000 μm²) taken with a beam of 2 × 2 μm² beam size, oxygen rich regions were chosen for the depth profile analysis. The investigated depth was ∼6 μm using particle detection (BS, NRA), which was extended to ∼11 μm with the application of the differential-PIGE method, using the numerical integration of experimental cross-section data. The oxygen depth profiles show systematic discrepancy in the oxide layer thickness and composition between the two different kind of shielding gases.
Evaluation of a setup for pNRA at LIBAF for applications in geosciences
2014, Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms
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The principle of pNRA is to analyze isotopic content of a sample by detecting both the gamma quanta and the charged particle produced in a nuclear reaction [4]. This technique was first proposed 20 years ago, it was suggested that it could be used for trace element analysis in thin samples [2] and depth profiling of thick samples [5]. The availability of many nuclear reactions for interaction of light ions with matter means that with the right choice of projectile and projectile energy all elements from lithium all the way up to chlorine can be observed and quantified [6].
A new setup for photon tagged nuclear reaction analysis pNRA is being developed at Lund’s ion beam analysis facility LIBAF. Particle induced gamma ray emission PIGE and nuclear reaction analysis NRA are two methods that have been extensively used for light isotope measurement in ion beam analysis IBA. There is an abundance of nuclear reactions between light elements and MeV protons, deuterons and alpha particles. This means that in principle all elements from lithium all the way up to chlorine can be analyzed using those techniques. Detection limits can be improved for some elements, if those two methods are fused together into pNRA.
The new setup for pNRA will benefit from advances in detector technology that occurred during the last 20 years. A LaBr₃ scintillator detector and an annular double sided silicon strip detector DSSSD are used in coincidence to detect a gamma and a charged particle respectively. Both detectors are connected to a VME based data acquisition system. Of primary interest in this work is the analysis of isotopic ratios of light elements in geological samples, which are usually thick with a complex matrix. This setup can be for instance used to measure isotopic fractionation of oxygen and boron. We will present the setup and discuss its capabilities.
Production and characterization of oxygen-reduced implanted <sup>21</sup>Ne targets
2009, Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms
Implanted neon targets were produced for nuclear astrophysics experiments at the Ruhr-Universität Bochum, and their characteristics were studied at the University of Notre Dame. The Ne ions were implanted sequentially at two different energies to create a more uniform depth distribution. The targets were stable under high beam loads. To reduce the amount of oxygen contamination on the target’s surface, a procedure of chemical cleaning and thermal outgassing of targets was developed. The impact of this treatment on implanted Ne targets was investigated and found to reduce the oxygen amount by a factor of 4. The depth profile of the implanted Ne atoms was studied via narrow (p, γ) resonances while the oxygen contamination was monitored using the Deuteron-Induced $γ$ -ray Emission (DIGE) method.
Depth profiling of carbon in silicon using the <sup>12</sup>C(p, p′γ) reaction
2008, Nuclear Instruments and Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms
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Analysis of oxygen and nitrogen in a sample including light elements is performed by detecting the protons and γ-rays from (d, pγ) reactions coincidently. Sensitivity for the detection of oxygen and nitrogen to the atomic ppm range can be achieved using this technique [2]. Coincident detection of a neutron and a γ-ray were applied for particle induced γ-ray emission (PIGE) measurements, and improvements of the sensitivity were reported [4].
An analytical method has been developed for the measurement of a carbon depth profile of the region a few tens of μm from the surface, using a ¹²C(p, p′γ) reaction. Measurements for a SiC sample coated with a silicon layer and a carbon-implanted silicon sample were performed using this method. Two charged particle detectors and two γ-ray detectors were utilized for the coincident detection of scattered protons and γ-rays from the first excited state (E_x = 4.4 MeV) of ¹²C. The measured depth profiles agree well with results obtained using a surface profiler and an Auger microprobe. These results demonstrate that this method is useful for the non-destructive analysis of carbon at depths of a few tens of μm from the surface.
Interaction of oxygen with nanocrystalline metals
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Nanocrystalline Ni and Fe specimens with a low oxygen content and mass-densities up to 98 and 93%, respectively, were produced by gas-phase condensation. The oxygen contents were determined by nuclear-reaction analysis (NRA) in the as-prepared state and after exposition to different oxygen partial pressures. NRA measurements in combination with serial sectioning by ion-beam sputtering show that the penetration of oxygen along open porosity is suppressed in the case of specimens with a high mass-density. Neither by NRA measurements nor by secondary-ion mass spectrometry (SIMS), performed after thermal treatments in oxygen in the temperature regime between 100 and 200°C, oxygen penetration can be detected in high-density nanocrystalline Ni specimens. This may indicate a low oxygen diffusion in interfaces of n-Ni. However, a low oxygen solubility may not be excluded.

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^∗: On leave from the Department of Physics, University of Arizona, Tucson, Arizona, USA.

^∗∗: On leave from the Physics Department, University of Pretoria, South Africa.

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High sensitivity analysis and profiling of oxygen and nitrogen by A (d, pγ)-coincidence technique

Abstract

Nucl. Instr. and Meth.

Nucl. Instr. and Meth.

Nucl. Instr. and Meth.

Nucl. Instr. and Meth.

Anal. Chem.