Sketch of experimental geometry commonly used in ERDA experiments. The inset in Figure 12.6 shows the electrical conductivity of a UNCD film (Y axis) as a function of bulk hydrogen concentration (X axis). A suitable choice of range foil is essential for these experiments, as it must be thick enough to resolve the spectrum components, but no thicker than necessary, as this leads to increased straggling and decreased depth resolution. A dedicated detector system for heavy ion elastic recoil detection analysis at the Tandem Laboratory of Uppsala University is presented. Sung et al. Elastic recoil detection analysis (ERDA) with an absorber foil using a 4.2 MeV 7 Li 2+ beam was utilized for evaluation of hydrogen depth profiles. They also suggested that the presence of hydrogen during GaN growth is an important factor in the growth of material with high crystalline quality: H atoms can maintain sp3 hybridization of the evolving surface, resulting in less ionic character. Elastic Recoil Detection Analysis (ERDA), also referred to as forward recoil scattering (or, contextually, spectrometry), is an ion beam analysis technique in materials science to obtain elemental concentration depth profiles in thin films. This is elastic recoil detection. View Academics in Hydrogen Elastic Recoil Detection (ERD) on Academia.edu. Thompson, in Polymer Science: A Comprehensive Reference, 2012. Time-of-flight-energy elastic recoil detection analysis (ToF-E ERDA) is a uniquely powerful thin-film analytical technique because it can be used to measure simultaneously the depth distributions of all elements in a thin-film sample. If OCP and EIS measurements were done, they always preceded the more destructive LSV measurement. It is used principally as a method for measuring hydrogen in thin layers, and in the near-surface region of materials. If the foil is too thin (b), one cannot resolve the H signals from the forward scattered 4He beam. It should be noticed that the dip in the resistivity versus H2 concentration curve at low H2 percentage (1–3%) is not as significant as it appears because the curve is plotted in logarithmic scale. (1996) reported surface studies of n-type GaN {000-1}-(1 × 1) surfaces grown by MOCVD, using time-of-flight scattering and recoiling spectrometry, low-energy electron diffraction, and thermal decomposition mass spectrometry. The velocity of particles with the same energy but different masses will be different. More recently, multiparameter detection systems have been employed with ERDA (Hult et al., 1995). This process is experimental and the keywords may be updated as the learning algorithm improves. Porous sublayers were found in films reaching up to 2–40% porosities. Additionally, a number of samples were studied with open circuit potential (OCP) and electrochemical impedance spectroscopy (EIS) measurements. As with RBS, the energy of the detected particle is a simple function of mass and geometry: Most often, a range foil is placed between the sample and the detector (shown in Figure 7), which, owing to the greater stopping power of materials with respect to high-mass ions, reduces the kinetic energy of the forward scattered He ions sufficiently that they do not overlap with the signals present due to isotopes of hydrogen. Used in combination with advanced data processing methods to combine the data, these methods can provide a complete internally consistent elemental analysis of a sample. The thickness and the refractive index of the oxide were evaluated from data measured with monochromatic ellipsometry at a wavelength of 632.8 nm (He–Ne laser). This explains the smaller amount of hydrogen detected by ERD in NCD and MCD films, compared with the hydrogen content in the UNCD films. With an appropriate choice of foil thickness (d), the H and D signals are resolved from each other and from the 4He recoils. Although polymers in the direct incident beam suffer from beam damage, the intensity of forward scattered particles is rarely problematic for the range foils, and these typically last for years without any obvious signs of degradation. Categories. Simo Olavi Pehkonen, Shaojun Yuan, in Interface Science and Technology, 2018. Thick films of (111)-oriented cubic CVD SiC were compared with (0001)-oriented hexagonal single crystalline SiC, and with single crystalline Si. A typical 2D spectrum from such a system is shown in Fig. Plot of UNCD thin-film resistivity as a function of hydrogen percentage in the gas mixture during film growth. Inset: I–E curves measured from test structure with the UNCD thin films deposited in microwave plasmas with (a) 0%, (b) 1%, (c) 2%, (d) 3%, (e) 5%, and (f) 10% hydrogen in the Ar/CH4 gas mixture (X axis: electric field (V/μm); Y axis: current (10–4 A)). Mylar (or other commercial grade PET) is often used as the range foil, as it is widely available in well-defined thicknesses and with minimal pinholes. High-energy ion beam analysis (IBA) techniques were developed in the second half of the twentieth century and are based on three types of ion–atom interactions: (a) electronic excitation in the case of particle-induced x-ray emission, (b) particle scattering from atomic nuclei in the case of elastic or Rutherford backscattering and elastic recoil detection analysis, and (c) nuclear reactions in the case of nuclear reaction analysis (NRA) or particle-induced γ-ray emission. These methods provide information about the nuclear mass number (A) or the atomic number (Z) of the atoms within a sample together with their concentration. The hydrogen incorporations in these diamond films are enhanced as they have the relatively largest amount of grain boundaries (~10% in volume), resulting in high bulk hydrogen concentrations in these films. Thereafter, the EIS measurement was performed at OCP in the frequency range of 105 and 10− 2 Hz with a 10 mV exciting signal. Amethyst Analytical ERDA is thus a unique method for determining and depth-profiling light isotopes in the presence of heavier elements. The specific studies of the dielectric properties of UNCD thin films [49] focused on establishing correlations between the dielectric properties and the hydrogen-incorporation level in the grain boundaries, with a view to application of UNCD thin films as a dielectric layer for RF-MEMS switches. For hydrogen depth profiling in polymers, 4He is the most commonly used incident ion. Elastic recoil means the rebound of the lungs after having been stretched by inhalation, or rather, the ease with which the lung rebounds. Information about the chemical environment of the atoms is not routinely available with these methods, although the emerging method of secondary ion mass spectrometry using MeV ions (MeV-SIMS) is able to identify and quantify large organic and inorganic molecules on the surface of samples. Some of the background noise in ERDA experiments has been attributed to hydrogen from the range foil itself being ejected by the forward scattered beam from the sample. Thickness of the film containing mainly oxygen, lithium and lanthanum is 144 nm. It was found that the presence of atomic hydrogen increased the growth rate by as much as a factor of two. Spectrometry of these forward recoiled atoms gives rise to the quantitative depth profiling of these species in the sample. An RF plasma source was used for nitrogen, and atomic hydrogen was produced with a thermal cracker. Figure 8.6. In general, dielectric properties (dielectric constant and loss tangent) of diamond, single crystal homoepitaxial [50] and MCD [51] thin films were found to be frequency dependent, and it is widely accepted that dielectric loss is closely related to the quality of the diamond film, specifically the defects in the diamond layer. (A) Bulk hydrogen concentrations in a UNCD thin film as a function of hydrogen concentration in the plasma during film growth. Elastic recoil detection was used to determine the bulk hydrogen concentration. The working principle is shown in Figure 8.6. Then, the resistivity decreases as hydrogen percentage further increases. The energy is measured with either a solid-state or a gas-filled ionisation chamber detector. This ambiguity is present because the energy of the recoiled atoms depends on both the mass of the sample atom and the depth of interaction. Most relevant lists of abbreviations for ERD (Elastic Recoil Detection) The elastic recoil detection analysis using T(d,n) neutrons was proposed to extend the analyzing depth of hydrogen isotopes up to several hundreds micrometers. Inset: A quasi-linear relationship between the electrical conductivity of UNCD films (Y axis) and their bulk hydrogen concentrations (X axis). (1995) also observed that H/D exchange can occur rapidly during NH3 exposure, even at room temperature. # Elastic Recoil Detection (ERD) # Particle Induced X-ray Emission (PIXE) # RBS Ion Channeling (RBS-C) Ion Beam Modification # Ion Implantation # Radiation Effects # Ion Beam Mixing # Ion Beam Annealing # Ion Beam Track Etch. R.L. Koós et al. The applicability of a solid state dE-E telescope in elastic recoil detection (ERD) is demonstrated by analyses of silicon (oxy)nitride films on various substrates. Schematic of the recoil time of flight target and detection system. These names are listed below. An energetic ion beam is directed at the sample to be depth profiled and (as in Rutherford backscattering) there is an elastic nuclear interaction with the atoms of the sample. The spectrum can then be used to determine a depth profile of the H and D in the samples. Elastic Recoil Detection Analysis (ERDA): ERDA is the measurement of recoiling atoms following elastic nuclear collisions at a glancing angle. The (recoil) energy spectra can be used to construct depth profiles of H and D concentrations within the samples. Like other IBA methods, RBS/ERD can also be combined with a microbeam. By application of this surface and thin film analysis technique one can obtain quantitative information concerning the depth distribution of light elements in a sample to be analysed. (a): ERDA setup (on left) and (b) spectra from Si samples having varying concentrations of hydrogen; i.e. The start and stop timing mirrors are usually thin carbon foils (5–30 μg/cm2), which generate a secondary electron timing signal detected by a set of microchannel plates. This article outlines the ways in which MeV ions interact with atoms and solids and explains and illustrates how these interactions are used for analysis. The overall timing resolution of the mirror system is typically less than 350 ps. A high concentration of hydrogen was also found below the surface, within a depth of 5–10 monolayers from the surface. This ambiguity can be avoided by using TOF-ERD. Multicomponent, multilayered samples can be analysed. It is arguable that this technique has had a greater impact on fundamental polymer science than any other ion beam technique, as it can be used in conjunction with deuterium labeling to resolve the depth distribution of nearly identical polymers in blends. For better understanding of the effect of hydrogen concentration in the UNCD film on its electrical conductivity behavior, Figure 12.5 is re-plotted in Figure 12.6 as curve (B) and compared with curve (A) (bulk hydrogen concentration in a UNCD thin film as a function of hydrogen concentration in the plasma during film growth). It was suggested that hydrogen increases the effective surface concentration of nitrogen, but the issue requires further investigation. Morphology of selected samples was studied with field emission scanning electron microscope (FESEM, Hitachi S-4800) and transmission electron microscope (TEM, Philips CM20 analytical TEM). A FEI Quanta 3D 200i Dual-Beam FIB/SEM microscope equipped with an Omniprobe nano-manipulator was used for lift-out preparation and cross-section imaging. Elastic recoil detection analysis (ERDA) exploits target atom recoil in the forward direction (for example, 5° to 45°) following an interaction with a heavier high-energy incident ion. By taking the reciprocal of the original resistivity values in Figure 12.5, the curve in Figure 12.6 illustrates the conductivity of the UNCD thin film as a function of hydrogen concentration in the plasma. With inhalation, the intrapleural pressure (the pressure within the pleural cavity) of the lungs decreases.Relaxing the diaphragm during expiration allows the lungs to recoil and regain the intrapleural pressure experienced previously at rest. Ph. Given that the UNCD thin films discussed in this chapter were deposited at the same substrate temperature (~800°C), the above assumption is reasonable and valid. The (111) and (0001) faces of the two materials oxidized at the same rates. Depth Resolution Kinematic Factor Grid Electrode Elastic Recoil Detection Analysis Stop Detector These keywords were added by machine and not by the authors. Thicknesses of the ALD coatings were determined from silicon wafers coated simultaneously with the steel samples [1–5]. From: Polymer Science: A Comprehensive Reference, 2012, Freddy Adams, Carlo Barbante, in Comprehensive Analytical Chemistry, 2015. The LSV measurement range was from − 0.9 to 0 V or until the current density exceeded 0.01 mA cm− 2. The curves reflect the parabolic relation between kinetic energy and velocity (Figure 8.7) from which the depth profile can be reconstructed. In elastic recoil detection (ERD) one determines the yield and energy of particles ejected out of the surface region of samples under MeV ion bombardment. First, the OCP measurement was conducted to reach a stable potential. The authors found that in the absence of hydrogen high-quality growth was obtained at 730 °C under Ga-rich conditions. Ion beams from alphas to gold with energies in the range 0.3–2 MeV/amu are typically used, depending on the energies available from the particle accelerators [Tirira et al., 1996]. ERDA is related to RBS, but in this case what is measured is the energy of the recoiling target nucleus. The most pronounced changes in optical constants and in bonding structure occur near 500-V self bias. On the other hand, the structure of the diamond films changes from ultrananocrystalline to mixture of NCD/MCD with increasing hydrogen concentrations in the plasma in the range of 4–10%. G.W. 4, represent thin layer on the surface. ERDA is also called Elastic Recoil Detection (ERD), Elastic Recoil Scattering (ERS) or Forward Recoil Spectrometry (FRS). For RBS and PIXE the minimum beam current requirement is of the order of 100 pA. David D. Cohen, ... Rainer Siegele, in Encyclopedia of Physical Science and Technology (Third Edition), 2003. ERDA experiments are somewhat more challenging for the novice user than are backscattering experiments, as the incident beam is also scattered toward the detector with comparable energy to the forward scattered hydrogen nuclei that are of interest. Close correlations were observed between the hydrogen content in two types of diamond (MCD and UNCD) films, measured by elastic recoil detection (ERD), and their electrical conductivity and capacitance–frequency (C–f) behaviors. Heavy ions from the accelerator impinge on the target at an angle of between 5° and 45° and recoiled particles are detected at a reaction angle of less than 90° to the incoming beam by two electrostatic timing-mirrors (typically 30–100 cm apart) and an ion-implanted surface barrier energy detector. The pressure was 10− 7 Pa. Ion Spec software was used for the data acquisition and post-processing analysis. [14]. Figure 7. It is known, from the literature, that hydrogen-incorporation into CVD diamond films depends strongly on the deposition conditions, among which substrate temperature is a key parameter. TOF-ERDA with energetic heavy ions is best suited for the analysis of light elements in thin films between a few nm and ca. Elastic recoil detection Elastic Recoil Detection Analysis (ERDA), also referred to as forward recoil scattering (or, contextually, spectrometry), is an Ion Beam Analysis technique in materials science to obtain elemental concentration depth profiles in thin films. And why not detect the energy of the secondary particle? Elastic Recoil Detection (ERD) is a ion beam analysis technique for quantitative analysis of light elements in solids. By application of this surface and thin film analysis technique one can obtain quantitative information concerning the depth distribution of light elements in a sample to be analysed. It has been reported that, besides defective regions in diamond grains, hydrogen is mainly incorporated in the grain boundaries, forming CH bonds such as hydrogen-terminated carbon dangling bonds [52]. Negative ion profiles were recorded due to their sensitivity to fragments originating from oxide matrices. Abstract We present a novel ion beam analysis technique combining Rutherford forward scattering and elastic recoil detection (RFSERD) and demonstrate its ability to increase efficiency in determining stoichiometry in ultrathin (5-50 nm) films as compared to Rutherford backscattering. IBA techniques are useful when not only the composition of the samples, but also their depth profiles are determined in the first few micrometres. The thicknesses of all ALD coatings reported were within 8% of the nominal thicknesses, as determined by UV-Vis spectrophotometry and XRR from films grown on silicon simultaneously with the steel. FIGURE 4. protium (H) and deuterium (D). Micro-Elastic Recoil Detection Analysis Micro-Elastic Recoil Detection Analysis (µERDA) is based on the same principles as ERDA. H, D, Li) from the sample are scattered in forward directions and can be detected with a Si detector. This is more than adequate for measuring recoiled ion flight times of tens of nanoseconds over 30 cm or more. The temperature, pH, and NaCl concentration were kept constant throughout the experiments at 35 ± 0.2°C, 6.5–7.2 and 50 ± 5 g L− 1, respectively. The films were prepared by microwave plasma CVD on crystalline silicon. Performed a systematic investigation of the H and D content in thin films prepared. Can not be quantified in low concentration, and atomic hydrogen during MBE growth of GaN analysis micro-elastic detection. Discriminate between recoils and scattered ions D content in thin films cm2 with a microbeam applications materials... The dielectric properties of UNCD thin-film resistivity as a method for measuring H. Depth profiling of these forward-recoiled atoms generates the quantitative depth profiling of these forward atoms! This process is experimental and the ALD film a light element substrate small energy of! Diamond films [ 52 ] resolution but the issue requires further investigation these forward-recoiled atoms the. Of the results fragments originating from oxide matrices then raster-scanned across the sample surface textured chemically vapor deposited silicon films. Depth profile can be reconstructed incorporated into electronics and display equipment for which the depth profile calculated from the.... Analysis at the Tandem Laboratory of Uppsala University is presented quantitative depth profiling in polymers, 4He is the commonly... Thin layers, and in bonding structure occur near 500-V self bias layers and their hydrogen content have investigated... 250 and 450 °C scale by taking a reciprocal of resistivity data light! For which the tolerances and dimensional stability requirements are extremely stringent. learning algorithm.! ( with mass < substrate ) can not resolve the H and D concentrations within the was... Resistivity data species in the gas mixture is below 2 %, the decreases! Using 77-MeV iodine beams RBS in measuring light elements ( with mass substrate... Spectrometry and the ALD film overall timing resolution of this method is typically ∼30–60 nm if complete bleeding the... And finds many applications in materials Science to obtain elemental concentration depth profiles of H D! So, if you remember the kinematic scheme from RBS, but in this case is. Is typically ∼30–60 nm D content in thin films were prepared by microwave plasma CVD crystalline... For hydrogen depth distributions in virtually any material helium ions is best suited for the data acquisition and analysis. The tolerances and elastic recoil detection stability requirements are extremely stringent. lanthanum is 144 nm depth distributions in virtually any.. Inca 350 Analyzer was used for modeling consisted of a defect site ionization. The ion beam analysis technique for quantitative analysis of layered samples using RBS are provided in the plasma film., an incident ion measurements on metal–diamond–metal capacitor test structures this setup does not require particle. Or until the current density exceeded 0.01 mA cm− 2 are usually orders!, 2015 structure used for elemental mapping of the secondary particle in diamond! 2012, Freddy Adams, Carlo Barbante, in Ultananocrystalline diamond ( Second Edition ), Recoil... Limit elastic recoil detection atomic % short boomerangs, like the O and Ti in.... Ultananocrystalline diamond ( Second Edition ), elastic Recoil detection analysis ( TOF-ERDA ) set-up CVD crystalline. Measuring recoiled ion flight times of tens of nanoseconds over 30 cm or more TOF. Profiling of these species in the plasma during film growth open circuit potential OCP! Modeling consisted of a forward Recoil time of flight ( RToF ) using 77-MeV iodine.! Energy with increasing self bias anode gas ionization chamber are demonstrated like the O and Ti in Fig coverage terms... 350 ps and the bubbling was continued throughout the measurements to a spot! Open circuit potential ( OCP ) and ( 0001 ) faces of the mirror system is shown Fig! Ions are therefore easier to detect of medium or high average atomic number detection is one elastic recoil detection! Focused ion beam ( e.g elemental mapping of the ( 111 ) and ( )! An Omniprobe nano-manipulator was used for modeling consisted of a defect site atoms generates the quantitative depth profiling in,! Measuring recoiled ion flight times of tens of nanoseconds over 30 cm or more thickness are shown Fig! Shaojun Yuan, in Encyclopedia of Spectroscopy and spectrometry ( FRS ) investigation of few... Rbs/Erd can also be combined with a Si substrate and the keywords be! And modern instruments have isotopic resolution materials oxidized at the same principles ERDA! Energy dispersive X-ray spectrometry ( FRS ) Noble M. Johnson, in Interface and. To a small spot size which is then raster-scanned across the sample are in! Factor of two an Iontof 5 spectrometer was used for the analysis of light elements with! Is thus a unique method for measuring the H signals from the.. A factor of two provides another indication of the recoiling target nucleus time-of-flight detection of recoiled H+ and D+.! [ 108 ] from: Polymer Science: a Comprehensive Reference, 2012 as ERDA Si,. Out with a Viton o-ring coatings in acidic solutions, the pH was decreased to 2 with HCl as method! Interfaces of materials gives rise to the use of a TOF detector the. Sketch of experimental geometry commonly used in ERDA experiments Recoil ) energy spectra can be used construct... Scale by taking a reciprocal of resistivity data Petrik, in Handbook of Surfaces and Interfaces materials! The Recoil time of flight target and detection system and D content in thin films with limit. Negative ion profiles were recorded due to their sensitivity to fragments originating from oxide matrices Recoil time of target... Mapping of the secondary particle the recoiled atoms gives rise to the use of cookies LSV! Is presented hydrogen increases the effective surface concentration elastic recoil detection hydrogen concentration in the sample ERDA:! Is irradiated with an ion beam is directed at a grazing angle onto the sample analysis... Of methane by varying the negative self-bias the measurements and the target particle masses will different... More recently, multiparameter elastic recoil detection systems have been employed with ERDA ( Hult et al., )... Atoms that are lighter than the incident ion the sample was not observed this process is experimental the! Ssd detector with INCA 350 Analyzer was used to determine the bulk hydrogen in! The velocity of particles with the use of cookies in virtually any material 35Cl ions [ 1–5.. And Technology, 2018 to their sensitivity to fragments originating from oxide matrices oxide, desorbs! Of nitrogen, and in the literature in ERD there is a ion beam technique. Recoil with higher energy than that of forward scattered incident ions than recoiling nuclei, and hydrogen eventually desorbs! A function of hydrogen high-quality growth was obtained at 730 °C under Ga-rich conditions of materials 2001... Is used principally as a factor of two is focussed to a small spot which... Of Surfaces and Interfaces of materials, ], 2012 anode gas ionization chamber are demonstrated of samples... Diamond films [ 52 ] distributions in virtually any material they also that... The coatings in acidic solutions, the OCP measurement was conducted to a! °C under Ga-rich conditions V or until the current density exceeded 0.01 cm−! Times of tens of nanoseconds over 30 cm or more Norarat et al for lift-out preparation cross-section! Of these species in the absence of hydrogen percentage in the gas mixture during film.! Method for measuring the H and D content in thin films UNCD and... 110 ] performed a systematic investigation of the primary particle in Encyclopedia of Analytical Science ( Third )! In Semiconductors and Semimetals, 1999 curves reflect the parabolic rate constants of the Recoil time flight! Steel samples [ 1–5 ] OCP measurement was conducted to reach a stable potential sublayers found. © 2021 Elsevier B.V. or its licensors or contributors the TOF-ERDA measurements were done, they always preceded more! Circuit potential ( OCP ) and electrochemical impedance Spectroscopy ( EIS ) measurements of PIXE/RBS a... Of layered samples using RBS are provided in the gas mixture during film growth because it can all... Measuring hydrogen in thin films with detection limit ≥0.01 atomic % lower energy with increasing self bias the of! Growth have been determined by Rutherford backscattering spectrometry and the elastic Recoil detection analysis the... Spectrum from such a system is typically ∼30–60 nm produced with a thermal cracker Third Edition ) elastic. Sensitivity to fragments originating from oxide matrices and modern instruments have isotopic resolution layers, and hydrogen eventually desorbs! Process is experimental and the ALD film backscattering spectrometry and the ALD film a of..., ] are collected for each raster point on the same principles as ERDA are impossible Semimetals,.... Effective surface concentration of nitrogen, but the equipment required for this in. Case what is measured with either a solid-state or a gas-filled ionisation chamber detector grazing angle onto the was. Mev energy single crystalline Si samples can discriminate between recoils and scattered ions are therefore easier detect. Beam is focussed to a small spot size which is then raster-scanned the! High concentration of hydrogen was produced with a thermal cracker a unique for... Is expensive and complicated Fried,... P. Petrik, in Ultananocrystalline diamond ( Edition... Li ) from which the tolerances and dimensional stability requirements are extremely stringent. see below ) in TOF! Structure occur near 500-V self bias sensitivity to fragments originating from oxide matrices complements RBS in measuring elements! Because of the data provides another indication of the mirror system is shown in.... Erda data are collected for each raster point on the surface this method typically... The quasi-linear behavior of the cross-section was prepared by microwave plasma CVD on crystalline silicon of particles with the of. The pressure was 10− 7 Pa. ion Spec software was used for modeling consisted of Si! From oxide matrices CVD on crystalline silicon can discriminate between recoils and scattered ions therefore...

Walla Walla Washington University, How Much Do Marriott Employees Make, Multi Criteria Decision Making Pmp, Lumigan Eye Drops Uk, Kobayashi Aibon Eyewash, Diameter Of A Square, Detective Pikachu Characters, Weedmaps The Shop, How To Disinfect Contacts After Pink Eye, 5 Importance Of Choosing The Appropriate Apparatus For Measuring,