journarof

Journal of Nuclear Materials 191-194 (1992) 67-74

North-Holland nuclear
materials

Radiation-induced microstructural change in ceramic materials

C. Kinoshita
Dfpartment of Nuclear Engineering, Kyushu Ullil'ersity 36 Hakozaki 6-10-1, Higashi-ku, Fukuoka 812, Japan

What is the characteristic difference between radiation-induced microstructural changes in ceramic and metallic
materials? /\ review is given of the current state of knowledge regarding this question, Elementary properties, which are
indispensable for describing the displacement process, are described for ionic and covalent crystals. The structure of cascade
damage and its stability are described in terms of the effects of deposited energy densiW and electronic cxcitation as well as
the characteristics of ceramic materials. The characteristic behavior of the nucleation and growth process of defect clusters
in various ceramic materials irradiated with electrons, ions and neutrons, which have been observed mainly through
transmission electron microscopy, is also reviewed. This review also considers the. effects of irradiation which is concurrent
with an applied electric field, transmutation-produced gases and atmosphere, though little definitive work has heen done.

1. Introduction excitation and knock-on and/or kinetic processes.

Design studies for the International Thermonuclear
Experimental Reactor (ITER) have become more de-
tailed in recent years, and requirements and operating
conditions for ceramic materials have become clear [lJ.
Plasma facing components, various insulators and win-
dows are required to maintain magnetic, optical and
electrical integrity as well as structural integrity under
various irradiation conditions [2]. Design studies are
based on adopting existing matcrials and thercfore
concentrate on suppressing the neutron flux and the
ionizing radiation dose. However, it is still indispens-
able to confirm the reliability of materials in fusion
environments. Furthermore demo and commercial re-
actors will require the development of new materials
and the description of the physical mcchanisms respon-
sible for radiation effects in fusion environments. The
strategies and stages of implementation for the study
of fusion materials arc (n qualification of existing
materials, (2) development of novel materials and (3)
fundamental understanding of radiation effects. How-
ever, with the cxception of some components of ITER,
existing ceramic materials might not work in fusion
environments. Therefore, basic experiments for devel-
oping novel materials and for characterizing the physi-
cal mechanisms involved in radiation effects are re-
quired. These experiments will be facilitated by the use
of a wide variety of well characterized irradiation facili-
ties.
The physical properties of ceramic materials re-
quired for use in fusion reactors arc related to the
electronic states of the constituent atoms, the atomic
configurations, and the overall microstructure, includ-
ing defect clusters. Radiation induced microstructural
changes in ceramic materials occur through electronic
These processes are dependent on several characteris-
tics of these materials, such as the atomic bonding, the
crystal structure, the mass of the constituent elements,
the impurity concentrations, the structural vacancy
concentration, and the grain boundary struclure: among
others. Therefore, it is critical that structural and prop-
erty changes be measured during irradiation rather
than after irradiation.
A review is given of the current state of knowledge
of the prominent features of radiation-induced mi-
crostructural changes in ceramic materials, in contrast
with those in metals. Included arc: (n fundamental
properties of atomic defects, such as the configuration
and the recombination volume of a Frenkel pair, the
displacement thrcshold energy and the migration en-
ergy of atomic defects in ionic (e.g. MgO) and covalent
(e.g. graphite and I3-SiC) crystals; (2) the effects of
deposition energy density, electronic excitation and low
energy knock-ons on the structure and the stability of
cascade damage; (3) the characteristic behavior of the
nucleation and growth process of defect clusters in
terms of the characteristic features of ceramic materi-
als; and (4) the effects of irradiation concurrent with
an applied electric ficld, transmutation-produced gases,
biased displacements of constituent elements and/or
atmosphere on the microstructural change. Descrip-
tions of the electronic structural changes are beyond
this review and are related to the irradiation-induced
property changes [3].
2. Fundamental properties of atomic defects
The displacement threshold energy, the defect con-
figuration, the formation energy, the recombination

0022-3115/92/$05.00 © 1992 - Elsevier Science Publishers B.Y. All rights reserved

68 C. Kinoshita / Radiation-induced change in ceramics

,..

rJf
H
CD

y
?T ,..
'(
}---<

z=L.!.
2

1
'10
( .r--'
CD
(b) H r0-

Y '-'
Mg 0

Fig. 1. The most stable configuration around an O-interstitial at (t t t) (a) and its spontaneous recombination sites marked with.
(b). The nearest neighbor Mg- and O-ions move, respectively, inward and outward along the (111) directions by 4.6% and 27.4%
[4].

volume and the migration energy of a Frenkel pair are The configuration of an interstitial on the basal
the most fundamental properties which are directly plane of graphite and its relative self-energy were
related to radiation-induced microstructural changes. determined [5] and they are shown in fig. 2. Covalent
Ceramic materials are generally regarded as either crystals have a wide variety of stable positions includ-
ionic or covalent crystals and are characterized by the ing pseudo-stable topological positions in contrast to
long range Coulomb interaction and the directional the definitive stable position in ionic crystals [4].
interaction in the respective crystals. The fundamental
properties of MgO [41 and graphite crystals [51 as
studied through the molecular dynamics (MD) tech- G - - - - ......-______e
nique are used as being representative of ionic and /
/
/
covalent crystals. Not only arc they candidate materials / /
/
/
for fusion reactors,but they have been also systemati-
cally studied (e.g. refs. [6-81). \
\
\
\
Fig. 1 shows a unit cell of MgO, containing an anion \ \

o
\ \
interstitial [41. The most stable anion interstitial is G-----(4t)---.....
configured at the body centered position, and in this (a)
configuration the nearest neighbor cations move in-
ward by 4.6% and the nearest neighbor anions move ~
outward by 27.4%, due to the Coulomb force. The ~
spontaneous recombination sites of the interstitial ion ffi .01
are also shown in the figure. A Frenkel pair along the ~
(110) directions is unstable, but stable along the (100)
!OO
directions showing alternative anion and cation ar-
a: '------'B7, ----'-;A'-O-A--:OA.:'-:,A".-B,,;.,'::.B-;;-----'
rangements. Surprisingly, the number of the recombi-
POSITION IN HEXAGONAL LATTICE
nation sites is 52, which is only 50% larger than that of
fcc metals [4]. In the case of an anion vacancy, the (b)
nearest neighbor Mg- and O-ions of the vacancy move Fig. 2. Possible sites of an interstitial located between two
outward along the (100) directions and inward along c-layers of hexagonal graphite and relative self-energies of the
the (110) directions by 11.1% and 5.5%, respectively, interstitial at possible sites. The atomic configuration of inter-
again due to the Coulomb force in contrast to the stitial positions such as N, N', Nil, B', B" and Bill is projected
inward relaxation in metallic and covalent crystals [91. on the hexagonal lattice. Atoms. and 0 are in layers below
and above the interstitial, respectively.
 C. Kinoshita / Radiation-induced change in cemmics 69

Table 1 a reliable result that the value along the (110) direc-
The formation energy (Er ) of a mono-valent and a di-valent tion is much higher than that along the (100) direc-
Frenkel pair and the migration energy (Em) of di-valent tion. because of easy recombinations of Frenkel pairs
vacancies in MgO. The results through the molecular dynamic alo~g the <110) directions shown in fig. 1.
(MD) technique [4], the static calculation [10] and experimen-
EI-Azab and Ghoniem [15J determined the displace-
tal [11,12) are compared
ment energy threshold surfaces of Si and C atoms in
Di-valent point defects Mono-valent SiC using the MD technique. Average displacement
point defects energies are 92.6 eV and 16.3 eV for Si and C atoms,
E r leV) Em leV]
Er[eV] respectively.
Mg 13.11 1.98 MD Mg 18.26
13.14 2.06 static calc.
o 12.65 1.97 MD o 17.46 3. The effects of deposition energy density, electronic
12.61 2.02 Static calc. excitation and low energy knock-ons on the structure
2.03±O.17 Experiment and the stability of cascade damage

When crystals arc irradiated with fast neutrons, the

The next properties discussed are the formation
energy of a Frenkel pair and the migration energy of
vacancies in MgO. Results on these properties deter-
mined through the MD technique [4], static calcula-
tions [10], and experiments [11,12J arc shown in table 1.
The migration energy of divalent oxygen vacancies is
1.97 eV as determined by the MD technique and 2.03
eV as determined by our experiments. The migration
energy of mono-valent point defects, however, might
be much different from this value, because the forma-
tion energies of a di-valent Frenkel pair and of a
mono-valent one are much different from each other
[4J. This feature cJlanges the kinetic behavior of point
defects under an ionizing radiation field.
The final property discussed is the temperature
dependen~c of the displacement threshold energy in
MgO. Fig. 3 shows experimental results presented by
Pells [13] and Satoh et a1. [11] together with results
obtained through the MD technique. The threshold
energy increases with decreasing temperature as also
seen in metals [14]. Because of the uncertainty in the
potential energy, the absolute values obtained through
the MD technique might not be reliable. However, it is
250
kinetic energy of the neutrons is transferred to primary
knock-on atoms (PKAs). One of characteristic features
of neutron irradiation is the cascade damage produced
by high-energy PKAs. It is possible to use energetic
ions combined with high voltage electron microscopy
(HVEM) to provide in situ observation of electronic
excitation and/or ion implantation [16-18] under im-
pulsive energy deposition. Abe et al. [18] found tiny
vacancy-type clusters corresponding to cascade damage
in Si, Ge, and a Si-Ge alloy under irradiation with a 30
keY Xe + ion flux of 1 X 10 15 Xe + /mzs. The visible
cluster density increased rapidly during the few sec-
onds of irradiation. In MgO, uAl 2 0) and MgAl 2 0 4 ,
they observed no clusters corresponding to individual
cascades, but observed black dot-contrast due to inter-
stitial dislocation loops after irradiation up to a higher
flue nee level. In those ionic crystals, vacancy-rich cores
are not stable enough to induce distinct contrast, but
interstitial loops appear through the nucleation and
growth process. The materials that have been irradi-
ated with the dual (ion plus electron) beam are listed
in the paper by Abe et al. [18]. According to their
results, the materials which evolve contrasts corre-
sponding to cascades are limited to covalent crystals
consisting of relatively high-Z elements. The amor-
phous phase appears in low-Z covalent crystals such as
graphite and SiC. Interstitial loops appear in ionic

200 & (110} Mg

L- (110) 0
Y}
: Palls ar al.
crystals. Concurrent irradiation with 30 keY Xe+ ions
and 1000 ke V electrons, which provide cascade damage
Molecular and only isolated Frenkel pairs, respectively, sup-
150 0 (100) 0 Dynamics @ Saleh &
presses the accumulation of cascade damage relative to
KlnosMa
t::. (100) Mg
that seen in experiments with single beam irradiation
Experiment
100 A with 30 keY Xe+ ions [18].
6 (110)Mg • (110) 0 Zinkie [19] observed an effect of concurrent dis-
(100)Mg
50 • (100) 0 (100) 0 placements and electronic excitation in the cross-sec-
@
tion microstructures of a.AlzO), MgO and MgAlZ04
0
0 200 400 500 800 1000 1200 following heavy ion irradiation at 650°C. Dislocation
Temperature (K) loop formation occurs only where the ionizing to dis-
Fig. 3. TIle temperature dependence of the displacement placive ratio is lower than about 10, 500 and 1000 for
threshold energy of Mg- and O-ions along the (l00) and MgAl 2 0 4 , MgO and aAl Z 0 3 , respectiveJy. ZinkJe
(110) directions in MgO [4,11,13). pointed out that the ratio of ionizing to displacive
70 C. Kinoshita / Radiation-induced change in ceramics
1 MeV Electron Irradiation
T· 77 K
0.5l !"n irrad. AI,o,
I ~~,cjJ
°1 2 3
PHOTON ENERGY ( eY )
4
Fig. 4. The optic.al density of photons emitted from virgin and
5
neutron irradiated aAl Z0 3 irradiated with 1000 keY elec-
trons for 1 f.LS at 77 K [20].
irradiation was one of the important radiation damage
parameters. The analogous behavior of loops was found
in MgAl204 irradiated with fission neutrons [6].
Tanimura and Hoh [20] found another synergistic
effect of displacement damage and electronic excita-
tion. Fig. 4 shows the optical density as a function of
photon energy for aA1 20 3 irradiated with pulsed 1000
keY electrons. Virgin aAl 20 3 emits small amount of
photons, but neutron irradiated aAl 20 3 emits large
numbers of photons corresponding to point defects.
4. The characteristic behavior of the nucleation and
growth process of defect clusters
Electron irradiation induces rather isolated Frenkel
pairs of interstitials and vacancies as well as electronic
excitation. Some of the point defects that escape re-
combination aggregate to fmm interstitial or vacancy
clusters. HVEM provides direct observation of the
nucleation and growth process of defect clusters during
electron irradiation. Various ceramic materials so far
observed have been classified into groups in terms of
the characteristics of the nucleation and growth pro-
cess of interstitial dislocation loops under electron
irradiation in HVEM [6,12]. The density and the size of
the loops were examined as functions of irradiation
time, electron flux, electron energy and irradiation
temperature. Fig. 5 shows typical examples of the vol-
ume density of dislocation loops in MgO, aAl 20 3 and
TiC o.85 as a function of irradiation time under 1000
keY electron fluxes of 0.9-2.0) X 10 23 e/m 2s at 0.30
Tm (Tm = melting point) [21]. In MgO, the volume
density of loops remains constant for increasing irradi-
ation time after the initial rapid nucleation. Irradiation
of aAl 2 0 3 with 1000 keY electrons gives linear nucle-
ation up to about 1000 s and then slower nucleation
eventually leading to saturation. The density of disloca-
tion loops in TiC o.85 , on the other hand, increases
linearly with increasing irradiation time after some
,. 3 0 , . . - - - - - - - - - - ,
1 a-AhO> ( 700K; 1.9 • JO:IJ elm~. )
j 25
~
:' 20
.
j"
J 2000
Time (sec)
3000
Fig. 5. Time dependence of the volume density of interstitial
dislocation loops in MgO, aAJ Z 0 3 and MgAlz04 during
irradiation with 1000 keY electron fluxes of (1.9-2.0) x 1O z3
e/m 2 s. Irradiation temperatures are shown in the figure and
about 0.3 Tm (Tm = melting point) [21].
incubation time for the times studied and may saturate
at higher fluences. Irradiation with 1000 keY electrons
induces no microstructural evolution in MgAlZ04 up to
the fluence level of 10 27 ejm 2 , except for the procduc-
tion of 'Y-alumina at temperatures above 1190 K [11].
Irradiation with 7 keY Ar+ ions, on the other hand,
induces nuclei of tiny loops which are mostly of the
i(111) interstitial type [6,11]. Instead of nucleating
dislocation loops, amorphization is induced at lower
temperatures in covalent crystals, such as graphite and
SiC [7,22].
The characteristic kinetic behavior of loops is based
on the size of the nuclei of the interstitial dislocation
loops. In ionic crystals, stoichiometric clusters lie on
definitive habit planes and the nucleus of the loop
might be anti-Schottky doublets for MgO, quintettes
for aAl z0 3 and septets for MgAlz0 4 , reflecting the
matrix structure in each case. In covalent crystals,
there might be a variety of topological configurations
of point defects and defect clusters, as seen in fig. 2,
especially at low temperatures. The structural vacancy
is another factor controlling the kinetics of loops.
TiC o.85 , for instance, contains 7.5% of structural vacan-
cies due to nonstoichiometry. Most of the displaced
atoms in TiC o.85 , therefore, can recombine with struc-
tural vacancies, and the nucleation and growth of inter-
stitialloops is greatly suppressed. The concentration of
interstitials contained in loops in MgO, TiC o.85 and
aA1 20 3 , expressed as a fraction of total atoms present,
is 1.8 X 10- 2, 6.0 X 10- 4 and 1.2 X 10- 3 after irradia-
tion to 4 X lO z6 ejm 2 (corresponding to about 0.5 and
1 dpa for MgO and aAl z0 3) at about 0.30 Tm , respec-
tively.
 C. Kinoshita I Radiation-induced change in ceramics 71
-1
;; 10
ture of loops in MgAl z0 4 . Three types of loops were
0I found; one was of the *(111) interstitial type which
~
I

""
.,;
-2
I
I was dominant at lower temperatures and lower fluence
.- 10 I
I levels. The other two were of the +(10) and the
--'- I
;a I
I ~(110) interstitial types seen at high temperatures and
~" I
0 high fIuences. Furthermore, {-(lIO) loops had three
~ I
-3 I
iI types of habit planes; these were the {Ill}, {1Ol} and
.
.~ 10
I

I
0- J
I
I
I {11O} planes. The fraction of
I
I
.~
I I
I I
"E I I
= ·4 I
~ 10 I
Fig. 6. The fraction of sUlvived Point defects comprising
"visible" dislocation loops per displacement per atom as
functions of irradiation temperature and neutron tluence [24],
for MgAl204.
Vacancy type clusters are generally voids, cavities or
bubbles. Colloid formation is a characteristic feature of
ionic crystals.
In order to confirm the general description, Ki-
noshita et al. [23] examined several materials such as
SiC, TiC o.85 , aAl Z0 3 and MgAl Z0 4 irradiated to fis-
sion-neutron fluences of 1 X 1O z 4, 1 X 10 25 and 9 X 10 z5
n/m z at 673, 773 and 873 K in Joyo, which is a fast
breeder testing reactor in Japan. Weak-beam dark-field
images of those materials irradiated at about 0.3 Tm
showed many tiny faint contrasts in SiC, reflecting a
wide variety of topological configurations of defect
clusters. Well-defined loops were observed in TiC o.85 ,
aAl z0 3 and MgAl Z0 4. Defect clusters in TiC o.85 ,
aAl z0 3 and MgAl z0 4 developed into interstitial loops
and tangled dislocations with increasing irradiation
temperature and fluence. The diameter and the den-
sity of the loops increased and decreased respectively
with increasing neutron tluence and irradiation tem-
perature. From the diameter and the density of loops,
the fraction of surviving point defects composing visi-
ble loops per dpa was estimated for all kinds of irradia-
tion conditions [21]. Although unfaulted loops and
dislocation lines also absorbed interstitials in a non-
conservative fashion, almost all loops in those crystals
irradiated at 673 K were faulted. As an example, the
results for MgAl Z0 4 [24] are shown in fig. 6. The
fraction is 0.002-0.09% for MgAlZ04' 0.06% for TiC o.85
irradiated at 673 K with a fluence of 1 X lO z4 n/m z
and more than 0.5% for aAl z0 3 irradiated under the
same condition. Recombinations with structural vacan-
cies provide a possible explanation for the lower inter-
stitial survival i.n MgAlZ04 and Ti.C o.8s .
In order to investigate other reasons for this sup-
pression, such as changes in loop nucleation and
growth, Kinoshita et al. [21] also determined the struc-
to
11) and t(1lO) loops
plotted as a function of the diameter of loops showed
t
that the loops change their character from the (111 )
type to the t(110) type during growth [21,24]. Among
the *(110) loops, smaller loops were on {Ill} planes,
middle ones on {lOll planes and larger ones on {11O}
planes [21,24J.
From those results, the character of loops is pre-
dicted to change according to the following steps: un-
stable tOl1) -> stable tOll) -> tOlO){ll I}
-> +(UO){llO} -> 1(l10){1l0}. The unstable loops dis-
appeared during TEM examination [6] and they are
predominantly detected after irradiation to lower neu-
tron fluences at lower irradiation temperatures. The
growth of some unstable (111) loops makes them
stable. During growth, dislocation loops change their
Burgers vector from -!;-(111) to t(11O) to reduce stack-
ing fault energy, and they further change their habit
planes from {111} to {IlO} planes through the rotation
of {Ill} planes along glide cylinders to reduce the
dislocation line energy [24].
The nuclei of t<llO){110} loops are as large as
anti-Schottky septets and their composition is stoichio-
metric MgAl Z0 4. Therefore, this type of loop has less
chance to nucleate. Loops of the *(111) type, on the
other hand, introduce both anion and cation faults and
a possible composition is Mg zAl04 or Al 3 0 4 . There-
fore, nuclei of these loops might be as large as septets,
but require no preservation of stoichiometry or electri-
cal neutrality. This type of loop has a greater chance to
*
nucleate than the (110) type does, though they are
not always stable under certain irradiation conditions.
In MgAl 2 0 4 irradiated with fission neutrons, no direct
nucleation of tOlO) type loops occurs, but t(111)
loops nucleate. The size of the nuclei are larger than
septets and some of the loops are unstable under
irradiation. These features might provide a lower prob-
ability of introducing stable defect clusters and explain
the radiation resistance of MgAl Z0 4 •
5. The effects of concurrent irradiation and electric
field, transmutation-produced gases and / or atmo-
sphere on the microstructural change
In this section, typical examples of the effects of
concurrent irradiation and electric field, transmuta-
tion-produced gases and/or atmosphere on the mi-
crostructural changes, which have been so far ob-
served, are shown.
72 C. Kinoshita I Radiation-induced change in ceramics

Fig. 7. A bright-field micrograph showing that He bubbles

prefrentially appeared at and near grain boundaries in SiC
ceramics containing B as sintering aid annealed at 1400°C for
1 h after irradiation at 640°C with fission neutrons to 6.0 X 10 24
n/m 2 (E > 100 keY) [32].
Hodgson [25,26] found serious electrical degrada-
tion in oxide insulators. Following a period of steady
conductivity due to induced electron-hole pairs, the
conductivity of aAI 2 0 3 increased exponentially during
irradiation around 500 C with 1.8 MeV electrons and
D
an applied electric field of 1.3 X 10 5 V 1m. Hodgson
pointed out the necessity of concurrent ionizing radia-
tion, displacement damage and electric field for this
degradation to occur, and found a marked similarity to
colloid production in alkali halides [27]. He also ob-
served large aluminum precipitates through optical mi-
croscopy, though no definitive mechanism of colloid
formation has been found.
Many workers have obtained results on the large
influence of He transmutation gas on cavity swelling in
Fig. 8. A dark-field micrograph showing the modulation of
aluminum colloids in OlAl Z0 3 irradiated at 650°C with 2000
keY AI + ions to 3.8 X 10 21 Al + 1m 2. The irradiated specimen
was examined in cross section with transmission electron
microscopy. EOR corresponds to the end of range of those
ions in OlAl z0 3 (19).
ceramic materials (e.g. ref. [28]). Iseki and his cowork-
ers [29-32] systematically studied the microstructural
evolution of radiation damage in SiC after neutron
irradiation and the subsequent annealing, using three
types of commercially available SiC ceramics, such as
reaction-bonded SiC containing free Si, pressureless
sintercd SiC containing 1% Band C, and hot-pressed
SiC containing 1% BcD. Among those ceramics, only
the SiC containing B evolved large He bubbles, shown
in fig. 7. This was accompanied by a large amount of
swelling through the nuclear reaction of 10B(n, arLi
and the sufficient flow of both He atoms and vacancies

Fig. 9. Bright-field micrographs showing dislocation loops or cavities in MgO irradiated at about 1200 K with 1000 keY electrons.
(a) and (b) are for MgO specimens rinsed in cold water and hot water for a few minutes, respectively.
 C. Kinoshita / Radiation-induced change in ceramics
to grain boundaries at temperatures above 1300°C. The
characteristic influence of H, He and C on microstruc-
tural evolution, such as loop formation, cavity forma-
tion, chemical change, in various ceramic materials is
also shown in these proceedings [33-38].
Biased displacements of constitucnt clements might
induce not only microstructural change but also chemi-
cal change due to the electro-chemical gradient. Fig. 8
shows aluminum colloids that are periodically modu-
lated in aAI 20, irradiated with 2000 keY Al+ ions up
to 3.8 X 10 21 Al +1m 2 at 650°C. This material was ex-
amined in cross section with transmission electron mi-
croscopy by Zinklc [19]. Preferential aluminum colloids
can be casily understood [38], but the modulation of
aluminum colloids, which was also obscrved after 1000
keV electron irradiation [11], might not be understood
without considering the effects of concurrent irradia-
tion and an electro-chemical gradient.
An example of the effects of concurrent irradiation
and atmospheric change is shown in fig. 9 [8]. It shows
dislocation loops or cavities in MgO first rinsed in cold
or boiling water, respectively for a' few minutes and
subsequently irradiated at about 1200 K with 1000 keY
electrons. Mg-vacancies might be introduced through
OH- ions present in boiling water and might combine
with irradiation induced O-vacancics to nucleate cavi-
ties.
6. Summary
A review is given of the current state of knowledge
of the fundamental material properties and processes
of radiation damage in ceramic materials. Examples of
characteristic phenomena of radiation-induced mi-
crostructures in ceramic materials are also given. The
future prospects lie in additional sophisticated experi-
ments to determine the response of these materials to
the expected fusion irradiation environment. Further
research is also needed to develop a better understand-
ing of the primary defect n:actions that givc rise to
property changes.
Acknowledgements
The author thanks Prof. N. Itoh, Dr. S.l. ZinkIe and
Dr. E.R. Hodgson for permitting the use of their
unpublished results, and Dr. T. Yano for preparing a
micrograph.
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