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Electrical Properties of a Semiconducting Layer Formed on SrTiO3 Single Crystal by Excimer

Laser Irradiation

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1999 Jpn. J. Appl. Phys. 38 894

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Jpn. J. Appl. Phys. Vol. 38 (1999) pp. 894–898
Part 1, No. 2A, February 1999
°1999
c Publication Board, Japanese Journal of Applied Physics

Electrical Properties of a Semiconducting Layer Formed on SrTiO3 Single Crystal

by Excimer Laser Irradiation
Jong-Won YOON and Masaru M IYAYAMA1
Research Center for Advanced Science and Technology, The University of Tokyo, 4-6-1 Komaba, Meguro-ku, Tokyo 153-8904, Japan
1 Department of Applied Chemistry, School of Engineering, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656, Japan

(Received March 25, 1998; accepted for publication December 1, 1998)

Effects of excimer laser irradiation on electrical properties were investigated for insulating SrTiO3 single crystals, and
the mechanism was discussed. A drastic drop of surface resistance from >1013 Ä/cm2 to about 104 Ä/cm2 was observed
after irradiation by KrF and XeCl laser light with fluences of about 100 and 200 mJ/cm2 , respectively. For laser irradiation
with a fluence above these critical values, the surface resistance remained at almost the same, low values. Traces of local
melting, in the form of microcracks, were recognized on the surfaces with low resistance. The low-resistance surface had n-
type semiconductivity, and the resistivity, electron concentration and mobility were estimated to be 0.2 Äcm, 5.4 × 1018 cm−3 ,
5.4 cm2 V−1 s−1 , respectively, by the Hall coefficient measurement assuming a semiconductive layer thickness of 0.3 µm. On the
basis of the result of X-ray photoelectron spectroscopic analysis, the drastic decrease in resistivity is attributed to the generation
of oxygen vacancies.
KEYWORDS: excimer laser, strontium titanate, semiconducting properties, oxygen vacancy, XPS analysis

field of microelectronic devices. Strontium titanate is an elec-

1. Introduction
Laser-induced processes on the surfaces of solids, includ-
ing laser annealing, photochemical etching and laser ablation,
have been topics of general interest. Laser etching has be-
come a topic of considerable interest in the area of microelec-
tronics, since this technique can be used for a variety of types
of circuit patterning. The laser ablation method has been used
for the production of thin films of ferroelectrics1, 2) and super-
conductors.3, 4) It has been established that the ablation pro-
cess depends on the wavelength, fluence and pulse width of
the laser beam. Basically two mechanisms for laser ablation
of materials have been suggested: (1) surface bonds are bro-
ken due to the high density of electronic excitations caused
by the absorption of laser photons, and (2) atoms are emitted
due to thermal melting of the surface caused by intense laser
beam irradiation. The former emphasizes the fact that elec-
tronic processes play an important role in ablation, although a
temperature rise may occur simultaneously and make an ad-
ditional contribution. For the latter, it is assumed that damage
of the surface occurs as a result of melting due to local heat-
ing, although photons are absorbed primarily through elec-
tronic transitions. The laser ablation process of oxide single
crystals (MgO, SrTiO3 and LaAlO3 ) has been investigated ex-
perimentally and theoretically, and concluded to be due to the
thermal effect, by means of solving the one-dimensional ther-
mal equation taking into account effects of laser recoil pres-
sure and optical reflection by the molten layer.5) However, it
is also reported that for Al2 O3 , etching occurs at a relatively
low temperature below the melting point.6)
On the other hand, laser irradiation is known to modify the
electrical properties of the surfaces of ceramic materials. In
the case of the ferroelectric, insulating BaTiO3 , a drastic drop
in the electrical resistivity was observed on the sample surface
after KrF excimer laser irradiation.7) The laser-irradiated sur-
face of BaTiO3 showed semiconducting behavior, which was
attributed to lattice defects. However, studies on the charac-
terization of the laser-irradiated surface are insufficient and
the conduction mechanism is yet unclear. If these can be clar-
ified, the application of laser irradiation, i.e., control of the
surface electrical properties, will be greatly extended in the
894
trical insulator at room temperature. By changing the stoi-
chiometry or by introducing dopants, major changes in the
electrical conductivity can be induced. Reduced SrTiO3 has
been shown to exhibit both semiconductivity8–10) and super-
conductivity.11–13) In the present study, changes in the electri-
cal properties of SrTiO3 by excimer laser irradiation were in-
vestigated, and the mechanism was evaluated by surface anal-
ysis using X-ray photoelectron spectroscopy (XPS).
2. Experimental Procedure
Commercial single crystals of SrTiO3 with purity of
99.99% (Shinko Ltd.) were used in the present study. The
sample geometry was usually 10 × 10 × 1 mm, and the sur-
face roughness was controlled to within 3 nm. The surface
of the SrTiO3 single crystal was irradiated by a KrF excimer
laser at room temperature in air, operated at a wavelength of
248 nm (5.0 eV photon energy) with 20 pulses of 18 ns dura-
tion at a 1 Hz repetition rate. In order to investigate the depen-
dence on fluence of the surface resistance, the laser fluence
was varied from 50 mJ/cm2 to 600 mJ/cm2 . For comparison,
an XeCl excimer laser with a wavelength of 308 nm (4.0 eV
photon energy) was also used to irradiate the surfaces of the
SrTiO3 single crystals. The laser pulse width, pulse rate and
pulsed energy density were, respectively, 18 ns, 1 Hz and 50–
600 mJ/cm2 , and the laser irradiation was performed in air at
room temperature.
For the electrical measurements, two In–Ga paste elec-
trodes were painted on the laser-irradiated surface separated
by 1 mm. The current–voltage characteristics were measured
in the voltage range from 10−1 to 102 V at room tempera-
ture using a picoammeter with a programmable DC voltage
source (HP4140B). Hall coefficient measurements were per-
formed by the Van der Pauw method at room temperature
(HL5500PC). The surface morphology after laser irradiation
was observed by field emission scanning electron microscopy
(FE-SEM; Hitachi4200) and atomic force microscopy (AFM;
Digital Instrument Nanoscope IIIa).
The XPS spectra were obtained using a ULVAC PHI 5600
electron spectrometer equipped with a monochromatic Mg
Kα X-ray source (1253.6 eV) at 400 W. The pressure inside
 Jpn. J. Appl. Phys. Vol. 38 (1999) Pt. 1, No. 2A J.-W. YOON and M. M IYAYAMA 895

the analysis chamber was 10−11 Torr. In order to improve the
S/N ratio of the spectrum, scanning with 0.1 eV steps was car-
ried out ten times for the O 1s, Ti 2p and Sr 3d peaks and five
times for the C 1s peak. The spectra were collected at a take-
off angle of 45◦ . The binding energies were calibrated using
the C 1s (285.0 eV) peak.
etching, mechanical polishing or a thin coating of conducting
materials (Au, Pt, etc.), the exhibition of different contrast on
the fracture surface is assumed to be due to the formation of
a conducting layer. Therefore, we assumed that the thickness
of the semiconducting layer formed by irradiation was 0.3 µm
(as indicated by the arrows).

3. Results and Discussion 3.2 Electrical properties of the laser-irradiated surface

3.1 Surface observation The optical energy band gap of SrTiO3 is reported to be
SrTiO3 single crystals are transparent and exhibit very high 3.2 eV.17) The surfaces of the specimens were irradiated by
electrical resistivity (>1013 Äcm) at room temperature. The KrF and XeCl lasers with photon energy above the band gap
surface of SrTiO3 becomes blue after excimer laser irradia- of SrTiO3 . Figure 3 shows the dependence of the surface re-
tion with a fluence above 100 mJ/cm2 . For the SrTiO3 single sistance of a SrTiO3 single crystal on the fluence of the ex-
crystals reduced by annealing in H2 -containing atmosphere, it cimer laser at two different wavelengths, 248 nm (KrF laser,
is known that a broad visible absorption band appears, which 5.0 eV) and 308 nm (XeCl laser, 4.0 eV). A drastic drop in the
spreads toward the infrared region, and the crystal shows a surface resistance, from >1013 to 104 Ä/cm2 , was observed at
light blue or dark blue color.14) The change in color is be-
lieved to be due to the formation of lattice defects such as
oxygen vacancies. In the same way, defects are assumed to
be formed on the surface of the laser-irradiated crystals.
The surface morphologies of a nonirradiated region (A)
and irradiated region (B) are shown in Fig. 1. In the laser-
irradiated regions, ripples, microcracks, and craters were ob-
served. These types of microdefects are typically observed
after local melting.15, 16) The microdefects in the specimen
surface are formed due to the ejection of atoms during the
laser irradiation. To determine the fluence level at which lo-
cal melting occurs on the irradiated surface, we examined
the specimen surface after irradiation at fluences above the
threshold level. The higher the laser fluence (F200 < F300 <
F400 ), the greater the number of ripples and craters observed
by SEM and AFM. This indicates that the thermal effect is
enhanced by higher laser fluence levels, whereas no change
in the structure of the mirror-like surface was observed at flu-
ences below the threshold level. Figure 2 shows the fracture
surface of a specimen irradiated at a fluence of 300 mJ/cm2 .
The dark side (A) appears similar to the non-irradiated re- Fig. 2. Scanning electron micrographs of the fractured surface of a
gion in Fig. 1. Since the sample is not treated with thermal KrF-excimer-laser-irradiated specimen at the fluence of 300 mJ/cm2 .

Fig. 3. The dependence on fluence of the surface resistance for SrTiO3

Fig. 1. Scanning electron microgaphs of the sample surface: (A) upon excimer laser irradiation at two different wavelengths, 248 nm (KrF
non-irradiated region and (B) KrF-excimer laser-irradiated region. laser, 5.0 eV) and 308 nm (XeCl laser, 4.0 eV).
896 Jpn. J. Appl. Phys. Vol. 38 (1999) Pt. 1, No. 2A J.-W. YOON and M. M IYAYAMA

fluences between 100 and 110 mJ/cm2 for KrF excimer laser doubly ionized vacancy, Vo·· , with the two extra electrons be-
irradiation. In the case of XeCl laser irradiation, the drop in ing donated to the conduction band as follows:
surface resistance occurred at fluences between 200 mJ/cm2
O∗o ↔ 1/2O2 (g) + Vo·· + 2e0 . (1)
and 210 mJ/cm2 . The threshold fluence at which a drastic
drop in the surface resistance occurs, was found to be lower Based on the above conduction model and the similarity of the
for laser irradiation of higher photon energy. Optical proper- conduction behavior shown in Table I, the oxygen vacancy
ties of SrTiO3 , determined by means of ultraviolet reflection model can account for the observed variations in electrical
and absorption spectra, have been already reported;18) the ab- resistivity for laser-irradiated specimens at fluences above the
sorption coefficient increases about three times of magnitude, threshold.
with photon energy increasing from 4 eV to 5 eV, and reflec- As mentioned in the introduction, the photothermal effect
tivity increases from 20 to 26% with an increase from 3.5 eV and the photoexcitation effect are known to be mechanisms of
to 4.0 eV.18) For the case of MgO irradiated with the ArF laser laser ablation. Based on the results of surface observations of
(193 nm), the relationship between reflectivity and the molten laser-irradiated SrTiO3 surfaces with traces of local melting,
layer has been estimated, and it was indicated that the re- the process of oxygen vacancy generation is assumed to be
flectivity increases about four times of magnitude when the mainly due to the photothermal effects, i.e., the laser energy
molten layer 0.3 µm thick is formed.5) Therefore the differ- is instantaneously converted to thermal energy at the surface
ence in the threshold fluence inducing the surface resistance and then oxygen atoms are thermally vaporized. However, it
drop between KrF and XeCl laser irradiation is assumed to is reported that the photochemical etching could occur even
be due to the difference in both the absorption coefficient and at a relatively low temperature; the etching of sapphire by
reflectivity. However, accurate estimation of the threshold flu- a 193 nm ArF laser (6.42 eV) occurs with a temperature in-
ence is difficult from only the present results. crease of about 130 K just prior to ablation and 200–300 K
In order to examine the semiconducting properties of the just above the threshold fluence of ablation.6) Accordingly,
surface of SrTiO3 irradiated by the excimer laser above the the photoexcitation process, which is the dissociation, by ab-
threshold fluence, I –V characteristics and Hall coefficients sorption of the laser photon energy above the optical band
were measured. Figure 4 shows the log I – log V plot for the gap, of surface oxygen due to electronic excitation between
specimens irradiated by the KrF excimer laser with various the O 2p and Ti 3d bands may be included in the present
fluences ranging from 200 to 400 mJ/cm2 . In the plot, a lin- SrTiO3 .
ear log I – log V relation with the slope of 1 was observed
for all specimens. Table I shows the results of the Hall co-
efficient and resistivity measurements for the sample irradi-
ated by the KrF excimer laser at a fluence of 300 mJ/cm2 .
These values were calculated based on the determination,
from SEM observations (Fig. 2), that the thickness of the
semiconducting layer formed by irradiation was 0.3 µm. Ta-
ble I also shows the reported values for the SrTiO3 spec-
imens prepared under other conditions.8) The major carrier
was identified to be electrons from the sign of the Hall coeffi-
cient. The resistivity, mobility, and carrier concentrations for
the laser-irradiated specimen were 0.2 Äcm, 5.4 cm2 V−1 s−1 ,
and 5.4×1018 cm−3 , respectively. These values are consistent
with those for SrTiO3 doped with donors and reduced in vac-
uum at 1000◦ C.8) Therefore, the excimer laser-irradiated sur-
faces for fluences above the threshold have n-type semicon-
ducting properties, similar to reduced or donor-doped spec-
imens. For undoped strontium titanate, it was reported by
Pladino et al. that the primary defect between 825◦ C and
1525◦ C is the oxygen vacancy.19) Also, the large decrease in
resistivity for samples treated in vacuum at 1000◦ C was at-
Fig. 4. The log(I )– log(V ) characteristic curve of KrF-excimer-laser-
tributed to the oxygen deficit. Loss of oxygen from the lattice irradiated specimens at the fluences of 200 mJ/cm2 (squares), 300 mJ/cm2
to the gas phase occurs accompanied by the formation of a (triangles), and 400 mJ/cm2 (black circles), respectively.

Table I. Resistivity, Hall mobility of electrons and carrier density depending on the reduction conditions.

Resistivity (ρ) Mobility (µ) Carrier density

Conditions of sample preparation
Äcm cm2 /Vs electron/cm3
KrF excimer laser irradiation at the fluence of 300 mJ/cm2 in air 0.215 5.4 5.4 × 1018
0.05 wt% Nb-doped as grown samplea) 0.2 6.5 5.0 × 1018
Vaccum of 1 × 10−3 Torr at 1273 K, for 28 ha) 0.35 5.9 1 − 3 × 1018
The surface and probe electrodes were made of indium. The results were obtained by the Van der Pauw method at room temperature.
a) results from ref. 8.
 Jpn. J. Appl. Phys. Vol. 38 (1999) Pt. 1, No. 2A J.-W. YOON and M. M IYAYAMA 897

3.3 Surface analysis by XPS O 1s (Fig. 6), the Oα1 (532.3±0.3 eV) peak was shown to
Figure 5 shows the core level spectra, O 1s, Ti 2p and Sr be have increasing intensity with increasing laser fluence,
3d, for nonirradiated (a), and SrTiO3 specimens irradiated by whereas the OL (530.4±0.1 eV) and Oα2 (533.6±0.5 eV)
the KrF excimer laser with fluences of 100 mJ/cm2 (b) and peaks exhibited the same intensity for all three samples. The
300 mJ/cm2 (c). The binding energies (BE) of the three dif- assignment of Oα1 and Oα2 peaks is confusing; the reported
ferent O 1s components, obtained from curve-fitting, are pre- species for Oα1 are oxygen anions adjacent to an anion va-
sented in Table II and Fig. 6. The following two points have cancy23, 24) and adsorbed O2− 20–22, 25)
2 , and the species for the
been noted: (1) the splitting of the O 1s spectrum, and (2) the Oα2 peak are surface hydroxyl groups26) and adsorbed wa-
merging of the Sr 3d1/2 and Sr 3d3/2 peaks. ter.25) If the Oα1 peaks are related to surface adsorbates, the
The O 1s spectrum in Fig. 5 shows splitting of the peak into intensity should change in a similar manner to that of the C1s
a lower BE component designated as OL , and a higher BE peak which is attributed to oxygenated carbon species ad-
component designated as Oα . The Oα peak grew in intensity sorbed on the surface. The intensity ratio, I (laser-irradiated
with increasing laser fluence (F0 < F100 < F300 ). Splitting sample)/I0 (non-irradiated sample), was 1.4 and 2.0 for sam-
of the O1s spectrum has been reported for various oxide ma- ples irradiated at the fluences of 100 mJ/cm2 and 300 mJ/cm2 ,
terials with the perovskite structure. The reported spacings
are 1.5 to 2.7 eV for LaMO3 (M=transition metal),20) 3.0 eV
for LaCoO3 ,21) and 3.8 eV for La1−x Srx CoO3 .22) According
to the reports, the OL peak with BE near 530 eV is assigned
to oxide ions in the lattice, and the Oα peak with a higher
BE is suggested to be due to adsorbed oxygen. On the con-
trary, according to the results of molecular orbital calculations
for SrCoO3−δ , a subpeak with the higher BE intensity was
found to increase with increasing oxygen vacancy concentra-
tion.23) From this result, the origin of the subpeak observed
for La1−x Srx CoO3−δ was suggested to be due to oxygen va-
cancies. In the present study, the OL (530.4±0.1 eV) peak
could be assigned to lattice oxygen.
According to the results of curve-fitting of the spectra of

Fig. 5. XPS core-level spectra of O 1s, Ti 2p, and Sr 3d collected at a Fig. 6. O 1s curve-fitting spectra: (a) nonirradiated specimen and
take-off angle of 45◦ : (a) nonirradiated specimen, and KrF-laser-irradiated KrF-laser-irradiated specimens at the fluences of (b) 100 mJ/cm2 and (c)
specimens at the fluences of (b) 100 mJ/cm2 , and (c) 300 mJ/cm2 . 300 mJ/cm2 .

Table II. Binding energies of XPS spectra (eV)

Oxygen (1s) Titanium (2p) Strontium (3d)

Sample
OL Oα1 Oα2 2p3/2 2p1/2 3d3/2 3d5/2
(a) Nonirradiated SrTiO3 530.3 532.2 533.6 459.1 464.9 135.3 133.6
(b) SrTiO3 irrdiated by KrF excimer laser at the fluence of 100 mJ/cm2 530.4 532.3 533.5 459.0 464.8 135.6 133.9
(c) SrTiO3 irrdiated by KrF excimer laser at the fluence of 300 mJ/cm2 530.4 532.5 534.1 459.1 464.9 135.4 133.8
898 Jpn. J. Appl. Phys. Vol. 38 (1999) Pt. 1, No. 2A
respectively. On the contrary, the intensity ratio of C1s for
these samples was 1.2 and 1.3, respectively. Therefore, the
Oα1 peak can be considered to be related to oxygen vacan-
cies, and the Oα2 peak is to that related with surface adsor-
bates. In the present study, since information on the O 2p
band is not obtained, estimation of electron concentration us-
ing the present XPS result is difficult. However, the O 1s XPS
spectrum of laser (300 mJ/cm2 )-irradiated SrTiO3 shown in
Fig. 6 is similar to that reported for La0.6 Sr0.4 CoO3−δ .22) The
oxygen deficiency has been reported to increase with increas-
ing Sr-concentration and temperature,27) and to be 0.275 in
La0.5 Sr0.5 CoO3−δ at 1200◦ C in air.28) The electron concentra-
tion of the above material, estimated from the oxygen defi-
ciency and the doped-Sr concentration, is 4.5 × 1020 cm−3 .
Since the Hall coefficient measurement was conducted at
room temperature in air, the difference between electron con-
centrations in Table I and those presented above may be due
to the trapping of electrons by adsorbed oxygens as well as to
differences in component cations and the measuring temper-
ature. Although the electron concentration is different in the
above estimation for La1−x Srx CoO3−δ and the present study
for SrTiO3 , these data agree in that the XPS Oα1 peak and
electron concentration are large in a perovskite oxide with a
high oxygen deficiency.
As for the XPS spectra of the metal cations, significant
changes in the binding energy were not observed for either
the Ti 2p or Sr 3d peak, but the merging of the Sr 3d1/2
and Sr3d3/2 peaks was observed for the laser-irradiated spec-
imens. It is known that a merging of Ti 2p peaks can be
observed when Ti3+ and Ti2+ ions are contained in the Ti-
bearing oxides. Accordingly, the results in Fig. 6 suggest that
the oxygen vacancies generated by the laser irradiation are
associated with the Sr2+ ions and do not lead to an appar-
ent change in the valence of the Ti4+ ions. However, further
study is necessary to evaluate the relation between the laser-
induced oxygen vacancies and metal cations.
4. Conclusions
The surface resistance of an insulating SrTiO3 single crys-
tal decreased drastically up on excimer laser irradiation with
the fluence above 100 mJ/cm2 for a KrF laser and above
200 mJ/cm2 for an XeCl laser. Hall coefficient measurements
showed that the low-resistance surface was n-type semicon-
ducting, and the values of resistivity, electron concentration,
and mobility were close to the reported values for H2 -reduced
and donor-doped SrTiO3 .
From the electrical measurements and XPS, the lowering
J.-W. YOON and M. M IYAYAMA
of resistivity was concluded to be due to the generation of
oxygen vacancies and quasi-free electrons, attributed to the
release of lattice oxygens by laser irradiation.
Acknowledgment
This work was carried out with financial support from the
Research Foundation for Materials Science.
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