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2 57Mn (57Fe) Implantation Mössbauer Spectroscopy

2 57Mn (57Fe) Implantation Mössbauer Spectroscopy

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ossbauer spectrometer had two Si detectors placed in front of and behind the sample and a plastic scintillation counter

installed just before the sample chamber to obtain the energy distribution of the 57 Mn particles after the Al degrader by

performing time-of-flight measurements. Typical implantation energy and intensity were estimated to be about 20 MeV/

ossbauer spectrometer had two insertion sites for

nucleon and 5 Â 106 particles sÀ1, respectively. The in-beam M€

samples; one was for low-temperature measurements using a liquid He cryostat and the other was for higher

temperatures up to 1200  C using a poly-BN heater. 57 Mn nuclei were implanted into the sample through a tantalum

collimator with a f 30 mm aperture. A CdZnTe detector monitored the M€

ossbauer g-rays emitted from the sample

during the M€

ossbauer measurements. The HIMAC facility of the National Institute of Radiological Science in Japan has

recently become available for 57 Mn implantation experiments. HIMAC can supply more energetic 57 Mn beams with

implantation energies up to 250 MeV/nucleon so that 57 Mn atoms are widely distributed over several hundred

micrometers at depths of a few millimeters from the surface.

€ ssbauer g-Rays

3.2.2 Detector for 14.4 keV Mo

A PPAC [50,51], a gas-filled resonance detector, has been employed for obtaining M€

ossbauer resonance spectra. The

ossbauer g-rays. The

PPAC detects internal conversion electrons emitted after resonance absorption of 14.4 keV 57 Fe M€

ossbauer absorber, 57 Fe-enriched stainless-steel foil, and a

parallel plates in the PPAC are a cathode made of a 57 Fe M€

graphite anode. Avalanches occur by gas ionization in the gap between these plates. Since 57 Fe has a large internal

conversion coefficient of a ( 8.2 for 14.4 keV M€

ossbauer g-rays, conversion electrons have a higher measurement

efficiency than M€

ossbauer g-quanta. The PPAC is expected to have a high detection efficiency and a large effect-to-noise

ratio, since it is background free for nonresonant g-radiation. Octafluoropropane (C3F8) was used as the counter gas of

the PPAC. A gas control system was used to control the flow rate and pressure. The PPAC was operated stably over a

week, which is sufficiently long to measure a M€

ossbauer spectrum.

3.2.3 Application to Materials Science—Ultratrace of Fe Atoms in Si and Dynamic Jumping

The diffusion mechanisms of dilute Fe atoms in semiconductors are currently one of the most important topics in solidstate physics and related applications. Dilute impurity Fe atoms are generally thought to occupy only interstitial sites in Si,

resulting in rapid diffusion. Fe atoms usually contaminate Si via diffusion annealing and quenching from high temperatures

during fabrication of Si wafers. The nature of Fe impurities has been evaluated at low temperatures in such samples. The

nature of Fe impurities were then evaluated at low temperature in such samples that must contain differently distributed

and/or clustered Fe atoms.

ossbauer spectroscopy up to 1200 K in the RIKEN accelerator

Yoshida et al. [52–54] used 57 Mn-implanted 57 Fe M€

facility to elucidate the charge states, lattice positions, and diffusion mechanism of interstitial Fe atoms in single-crystal Si.

An n-type floating-zone Si wafer (6 Â 1018 As cmÀ3) with a thickness of 600 mm was used in this experiment. The Si

sample was fixed in a Ta holder and it was orientated at 45 relative to the beam direction (see Fig. 3.2). The


Mn-implanted 57 Fe M€

ossbauer spectrum was measured from low temperature to 1200 K. The total 57 Mn fluence was

12 57

Mn cmÀ2 in a spectrum (see Fig. 3.3). Spectra obtained between 300 and 700 K could be fitted by two

typically 2 Â 10

Lorentzian curves, whereas spectra obtained between 800 and 1200 K could be analyzed by a single broad singlet. The left

and right singlets have been assigned to 57 Fe atoms present at interstitial and substitutional sites in Si, respectively. This

assignment is based on a theoretical calculation of the center shifts [55]. The broken line shown in Fig. 3.3 indicates the

normal temperature dependence due to the second-order Doppler shift (SOD). Neither the interstitial nor the

substitutional components obeyed the SOD temperature dependence. This anomaly was accompanied by a reduction in

the area intensity. These observations clearly indicate that the 57 Fe atoms jump within the lifetime of the excited


ossbauer level, leading to a linewidth that is too broad to be fitted by a single Lorentzian curve. The area recovery above

1100 K suggests that the jump frequency of the 57 Fe atoms was suppressed due to a recombination reaction (such as

ossbauer diffusivity induced by 57 Fe jumps

interstitial 57 Fe atoms jumping into vacancies). This is a first observation of M€

from different lattice positions between interstitial and substitutional sites in Si. The activation enthalpy of an interstitial

Fe jump within the lifetime was estimated to be 0.67 eV from the measured temperature dependence of diffusion line


This experiment is extended to polycrystalline silicon. Polycrystalline silicon is widely used for solar cells, while it

contains different lattice defects. This type of experiment is important for improving the generating efficiency to

investigate the charge states and the lattice positions of Fe impurities associated with lattice defects produced by light

illumination and application of an external voltage.








€ ssbauer spectra of 57 Mn

Fe Mo

implanted in an n-type floatingzone Si wafer between 330 and

1200 K [54]. The isomer shift is

given relative to a-Fe at room

temperature and the sign of the

velocity is given in the emission

source experiment. (Reproduced

from Ref. 54 with permission of


3.2.4 Application to Inorganic Chemistry Unusual High Fe Oxidation States It seems impossible to experimentally prove the presence of higher

oxidation states of Fe atoms EC decayed from 57 Co because the lifetime of higher states produced by the Auger process

ossbauer level [56]. The aftereffects near the

is shorter than the M€

ossbauer time scale (t % 10À7 s) for the excited M€


probes caused by b -decay are not as serious as those produced by the Auger process in 57 Co. The oxidation states

produced in 57 Fe arising from 57 Mn through bÀ-decay are expected to have unusually high because Mn ions are more

stable in higher oxidation states, as generally known in solid-state chemistry.

ossbauer spectra of 57 Mn implanted into KMnO4 below 130 K. The Mn ions

Kobayashi et al. [57,58] measured 57 Fe M€

in KMnO4 are in a ỵ7 state and form a symmetric [MnO4] tetrahedra. The implantation energy and typical intensity

were evaluated to be 17 MeV/nucleon and 2 Â 105 57 Mn sÀ1, respectively. The obtained spectra could be analyzed by two

components consisting of symmetric doublets and singlets (see Fig. 3.4). The doublet was ascribed to a typical Fe2ỵ in a

high spin state, of which isomer shift and quadrupole splitting were not strongly dependent on the temperature up to

130 K. On the other hand, the isomer shift of singlet measured at 11 K was determined to be À0.38(5) mm sÀ1, suggesting

exotic Fe species in unusual valence states. The anomalous singlet is thought to produce substitutional Fe atoms in regular

Mn sites of [MnO4]À tetrahedra. The molecular orbital wave functions were calculated to estimate the relationship

between the oxidation states and the electron densities of Fe atoms in tetrahedral [FeO4]n. The Gaussian calculation

shows that [FeO4]2 (Fe6ỵ (3d2)) and [FeO4]0 (Fe8ỵ (3d0)) are the most stable geometries. The FeO bond tends to

become increasingly ionic with an increasing valence state of Fe so that the contribution of 3d electrons to the bonding

orbitals increases, while that to the antibonding orbitals decreases. Although the total population number of 3d electrons

of the Fe atom decreases with decreasing number of antibonding electrons from Fe2ỵ to Fe6ỵ, the population of 3d

electrons in the Fe atom increases due to the covalent character in the region from Fe6ỵ to Fe8ỵ. It is known that an

isomer shift of [FeO4]2, corresponding to Fe6ỵ, appears at 0.85 mm s1 in alkali oxoferrates [59,60]. Tetrahedral

[FeO4]0 of a high valence state is considered to have a lower isomer shift than alkali oxoferrates. The singlet was ascribed

to be 57 Fe atoms substituted for Mn sites in tetrahedral [FeO4]0 of a high oxidation state of Fe8ỵ.






€ ssbauer spectrum of

Fe Mo


Mn implanted in KMnO4 at

11 K. (Reproduced from Ref. 58

with permission of Springer.) Exotic Localized Fe Molecules Kobayashi et al. [61] have also performed in situ characterization of the

ossbauer spectroscopy. It is well

reaction products between Fe and solid oxygen by means of 57 Mn-implanted 57 Fe M€

known that solid O2 (mp ¼ 54 K) occurs in three phases at low temperatures: a-O2 (T < 24 K), b-O2 (24 T < 44 K), and

g-O2 (44 T < 54 K). It is considered that a- and b-O2 are antiferromagnetic, whereas g-O2 is paramagnetic. One

millimeter thick of solid O2 sample was prepared on an Al plate cooled by a liquid He flow. High purity O2 gas was

introduced around the sample plate to prevent sublimation caused by the vapor pressure of solid O2. The implantation

energy and intensity of the 57 Mn beam were estimated to be 26 MeV/nucleon and 5 Â 106 57 Mn sÀ1, respectively. The

stopping range of 57 Mn in the solid O2 was calculated to be 180 mm from the surface with a straggling range of Ỉ100 mm.

The total implantation dose of 57 Mn was typically 5 Â 1011 57 Mn cmÀ2 for one spectrum.

The obtained spectra were analyzed using four paramagnetic doublets (Fig. 3.5), based on earlier M€

ossbauer and

infrared measurements of an Ar matrix isolation of laser-ablated Fe atoms and of the reaction products with O2 gas at low



€ ssbauer spectra of 57 Mn

Fe Mo

implanted in solid oxygen at (a)

18 and (b) 32 K. (Reproduced

from Ref. 61 with permission of








Optimized molecular structures

of unstable Fe–O reaction products using ab initio Gaussian 03

program. Large circles are Fe

atoms and small circles are oxygen atoms. Bond lengths are

given in angstroms (A) and bond

angles (bold italic) in degrees.

(Reproduced from Ref. 61 with

permission of Springer.)

temperatures [62]. Figure 3.6 shows the optimized chemical species of FeO (S ¼ 2), Fe(O2) (S ¼ 1), (O2)FeO2 (S ¼ 0), and

ossbauer parameters and ab initio molecular orbital calculations using Gaussian 98/03

Fe(O2)2 (S ¼ 0) obtained from the M€

programs. Fe(O2)2 is formed in the 57 Mn implantation experiment and is also a major component of the resonance area at

all temperatures, for example, 49% at 18 K, 45% at 32 K, and 60% at 45 K.

Although an energetic 57 Mn atom will create defects and break up O2 molecules until it stops at a suitable final

position in the solid, an 57 Fe atom arising from 57 Mn at the final position will be surrounded by O2 molecules and the

initial reaction products generated during the lifetime of the excited M€

ossbauer level. Investigations of chemical reactions

using highly excited atoms may contribute to our understanding of both the production mechanism of the initial reaction

products and the chemical reactions in the ionosphere and interstellar space.

€ ssbauer g-Ray Detector

3.2.5 Development of Mo

Weyer [50] developed a conversion electron detector based on a PPAC for M€

ossbauer spectroscopy. Conversion

electrons are emitted from the surface of a M€

ossbauer absorber after resonance absorption with a conversion coefficient


a (a ¼ 8.2 for 14.4 keV 57 Fe). In principle, a conversion electron detector is very sensitive only for resonant M€

g-rays without interference of nonresonant g-radiations. The PPAC is important for in-beam M€

ossbauer spectroscopy of

implanted excited atoms and RI nuclei in environments with high backgrounds.

However, especially in 57 Mn implantation measurements, the effect-to-background ratio is typically of the order of

10%, which is much lower than that obtained in offline measurements using a 57 Co/Rh source. The electrons emitted by

b-decay of 57 Mn are thought to significantly degrade the spectral quality because the energy resolution of the PPAC used

was too low to distinguish conversion electrons from b-rays. Nagatomo et al. [32,33] have improved the effect-toossbauer spectra using a b–g anticoincidence method that employs a plastic

background ratio of 57 Mn-implanted 57 Fe M€

scintillation detector to detect and reject extraneous b-rays emitted from 57 Mn. In order to demonstrate the

effectiveness of the anticoincidence method, they performed M€

ossbauer spectroscopy of 57 Fe generated from the





Neutron capture in-beam

€ ssbauer spectrum of FeS2


(pyrite type) at room temperature. Measurement time was

70 h. (Reproduced from

Ref. 66 with permission of


b-decay of 57 Mn nuclei implanted into an Al plate at room temperature. By eliminating the extraneous b-rays, the

anticoincidence method drastically increased the effect-to-background ratio of the relative peak height above the baseline

from 10 to 220% (an approximately 20-fold increase). The newly developed anticoincidence detection system enables in

situ characterization of completely isolated atoms in a solid using a low implantation dose of 5 Â 108 57 Mn cmÀ3.



The chemical behaviors of hot atoms after nuclear reactions (e.g., (n, g) reaction) have been studied by radiochemical

researchers. The much higher excitation energy than conventional chemical reactions produces rare and anomalous

chemical species [63,64]. The chemical effects of hot atoms in gaseous and liquid phases are well understood, whereas

those in solid states are not so much. The chemistry of hot atoms in solids is critical for understanding the effects of

radiation on materials used in energy-production facilities. Neutron capture reactions are free from ionization generated

by charged particles and from charged particle emission, which inevitably decompose molecules and produce lattice

defects. Only cascade g-ray emission during relaxation from approximately 8 MeV excited levels imparts a recoil energy

to the nucleus involved in the reaction. The recoil energy is typically about a few hundred electron volts, which is an order

of magnitude larger than the lattice dislocation energy of atoms in solids. This allows the relaxation products of a highly

excited atom to be observed far from thermal equilibrium in the medium. A combination of (n, g) reaction and emission


ossbauer spectroscopy are very important for studying the chemical behavior of hot atoms. However, there have been

few reports of neutron in-beam M€

ossbauer spectroscopy [3–5]; this is probably due to the complicated detection system

required and the high background level.

Kubo et al. [65–67] recently demonstrated neutron in-beam M€

ossbauer spectroscopy with the aim of performing

detailed in situ investigations of the chemical behavior of trace Fe species formed by the 56 Fe (n, g) 57 Fe reaction. This

experiment was performed at the research reactor at JAEA. The thermal neutron flux was approximately 1.0 Â 108

n cmÀ2 sÀ1 when the reactor was operated at a thermal power of 20 MW. They used iron disulfide (FeS2: pyrite) as the

sample. Pyrite is a binary semiconductor and has a rock-salt crystal structure consisting of Fe2ỵ cations and S22 anions.

The obtained neutron in-beam M€

ossbauer spectrum of pyrite FeS2 was analyzed using two doublets at room temperature

(see Fig. 3.7). Component I has similar M€

ossbauer parameters to those of the parent pyrite, whereas component II has

different parameters. This indicates that the 57 Fe atom formed by the (n, g) reaction was removed from its original

position by the cascade g-radiation recoil and is in a different position from the original pyrite.

A Hungarian group [68] has recently commenced a neutron in-beam M€

ossbauer study using a cold neutron source

(flux of $109 n cmÀ2 sÀ1) and a guide system at the Budapest Research Reactor.


This chapter describes some past and current topics in in-beam M€

ossbauer spectroscopy. There have been a wide variety

of application-related studies of in-beam M€

ossbauer spectroscopy in conjunction with nuclear reactions, Coulomb

excitation, recoil implantation, and short-lived RI beams. New in-beam measurement methods and the introduction of



excited M€

ossbauer levels into materials for materials science and chemistry applications are currently being developed at

accelerator and neutron facilities. As mentioned above, the in-beam technique is a source experiment using M€


g-radiation emitted from the sample of interest. It is possible to detect extremely dilute concentrations of atoms and

their environments with a high sensitivity. The in-beam technique provides unique and unprecedented information on

dilute M€

ossbauer atoms in a material. In the field of materials science, in-beam M€

ossbauer spectroscopy enables

observation of the final position of dilute impurity atoms in semiconductors and atomic jumping. The time-dependent

dynamic behavior of single isolated atoms (not only atomic jumping but also the thermal stability and defect formation and

recovery) can be investigated by applying an appropriate time window. It is possible to form and analyze unusual chemical

species in exotic metastable states that are impossible to synthesize by normal chemical reactions. In-beam M€


spectroscopy is considered to be the only means available for characterizing in situ and directly observing chemical effects

produced by hot atoms prior to reaching excited M€

ossbauer levels. In particular, short-lived RI beams produced as

secondary beams from projectile fragmentation reactions and online mass separators are available at several laboratories

in the world. RI beams are becoming important in materials science and chemistry. Their intensities are increasing and the

implantation energies extend up to the gigaelectron volt region, which are several orders of magnitude higher than those

of conventional ion implantation techniques. Thus, RI beams can be applied not only as a M€

ossbauer probe for obtaining

atomistic information on processes occurring immediately after implantation, but also as an effective tool for producing

exotic chemical species and/or oxidation states. It is anticipated that in-beam M€

ossbauer spectroscopy will become more

and more useful in the fields of materials science and chemistry as it complements several conventional measurement






























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