Cuprous oxide-indium-tin oxide thin film photoYoltaic cells

Masaharu Fujinaka
Department of Electronics, Tokyo Denki University, Chiyoda-Ku, Tokyo 101, Japan

Alexander A. Berezin
Department of Engineering Physics, McMaster University, Hamilton, Ontario, Canada, L8S 4M1

(Received 25 June 1982; accepted for publication 14 January 1983)

We studied thin films of cuprous oxide deposited on glass coated with transparent conducting
indium-tin oxide (ITO) films. The deposition of both Cu 2 0 and ITO was made by rf sputtering in
an Ar/02 gas mixture. For the deposition ofCu 20 a pure copper target was used and ITO films
were deposited from a disk target, the halves of which were made ofSn and In, respectively. This
allows variation of the stoichiometry of the deposited ITO film by changing the position of the
substrate glass beneath the Sn/ln target. X-ray diffraction of Cu 20 films indicates the typical
pattern of amorphous material. We were able to produce Cu 20 films of different stoichiometry by
varying the O 2 to Ar ratio during rf sputtering. The maximum resistivity of the films corresponds
to an ideal stoichiometry ofCu 20. An activation energy of 0.55 eV found from thermostimulated
conductivity is related to excess Cu vacancies. The band gap found from the spectral dependence
of the photovoltaic effect is 2.0 eV. The composition of ITO films was studied by Auger analysis
and can be described as a variable composition mixture ofSn0 2 + x and In 20 3 + y' To produce an
Ohmic electrode, gold was evaporated on the top of the Cu 20 film and hence the resulting
structure of the photocell could be specified as ITO-Cu 20-Au, for which we propose a barrier
band diagram. We studied the photovoltaic characteristics of the fabricated photocells under an
incandescent lamp with ~ 100m W /cm 2 output. The open-circuit voltage and short-circuit
current of our cells were about 20-90 mV and 50,uA/cm2, respectively, and some dependence of
the output characteristics on the composition ofITO film was observed. Conversion efficiency for
thin films Cu 20/ITO cells was found to be substantially lower than for Cu 20/Cu Schottky
barrier cells. This is tentatively attributed to small diffusion lengths and/or presence of interface
recombination centers.
PACS numbers: 85.60.Dw, 72.40.

+ w, 73.40.Lq, 8U5.Cd

I. INTRODUCTION

Cuprous oxide (Cu 20) is considered to be a useful material for photo voltaic energy conversion because it has a proper band gap (~2.0 eV), high efficiency of generation of photocarriers and also because of its potential low cost. Cuprous
oxide thin films can be also produced by the same sputtering
technique as indium-tin oxide (ITO) films considered earlier. !
Most of the earlier studies of Cu 20 photocells included
Schottky barrier, MIS, and heterojunction structures based
on thermally prepared CU20 or electrodeposited Cu 20 (see,
e.g., Refs. 2-9 and references therein).
It is the purpose of this paper to report on the study of
the photocells of Cu 20 deposited on glass coated with transparent conducting ITO films! of different compositions. The
ITO can form a heterojunction with Cu 20 film 4 5 as well as
be used as a window material for solar radiation.
The deposition of both Cu 20 and ITO was made by
radio-frequency (rf) sputtering of metals in an Ar/02 gas
mixture. Some dependence of the output characteristics on
the composition of ITO film was observed.
II. EXPERIMENT

The schematic diagram of the apparatus used in this

work is shown in Fig. I. The basic sputtering system was a
Materials Research Corporation type 8551 rf sputter unit
3582

J. Appl. Phys. 54 (6), June 1983

with an oil diffusion pump system. The water cooled target

was 12.7 cm in diameter and the distance between the upper
and the lower cathodes was 9.2 cm.
After pumping down to a background pressure of
6 X 10- 6 Torr in the sputtering chamber, Ar and O 2 gases,
controlled by separate flowmeters, were mixed together in
the gas mixture chamber, and then introduced into the sputtering chamber through a gas leak valve. Then, we raised the
total pressure to the desired value of2.5 X 10- 3 Torr in order
to keep the discharge continuous and the plasma stable. The
target was sputter cleaned for a few minutes with a shutter
covering the substrates. Finally, the deposition was started
by moving the shutter.

III. ITO PREPARATION AND CHARACTERIZATION

The transparent conducting ITO films were deposited

by rfsputtering in the gas mixture of Ar (flow rate: 100 cm 3 /
min) and O 2 (flow rate: 20 cm 3/min) on cleaned micro slide
glass (Sargent-Welch Scientific Company).! The disk target
consisted of two semicircular parts which were made of Sn
and In, respectively (0.5 mm thick, 99.99% purity). This impurity level is probably not very important for the overall
resistivity of the film (it is basically dominated by the In to Sn
ratio), but it may be essential for the recombination processes
at the Cu 20/ITO interface. This finally can have a detrimen-

0021-8979/83/063582-07$02.40

1983 American Institute of Physics

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power
_ .....:..:..:.., supply
FIG. I. Schematic diagram of the apparatus
for the deposition of thin films by the radiofrequency sputtering system. (FM = flowmeters).

tal effect of a conversion efficiency (see Sec. VI). The deposition time was 18 min at an rf power level of 50 W.
The position (A,B ...F) of the glass substrates and the
relative sizes of Sn and In are shown in Fig. 2. Figure 2(a) is
for the case when the disk target consists of two equal halves
ofSn and In, respectively. Figure 2(b) is for the case when the
In side is substantially larger than the Sn side [see insert in
Fig. 2(b)]. We measured the electrical resistance, the Auger
signal, and the optical transmittance to evaluate the composition of the fabricated ITO films. 1
To measure sheet resistance of ITO films we used two
parallel evaporated gold electrodes of 5-mm length with 0.3mm gap between them (see the insert to Fig. 5 for the similar
arrangement). The measured sheet resistances are shown in
Fig. 2.
The resistance changes rapidly just beneath boundary
of Sn and In on the target. By moving the position of substrate glasses toward In side, the resistance can be decreased.
The observation of the energy spectra of Auger electrons emitted from the ITO films provides an effective tool

for the chemical analysis of the composition. The Auger

spectra of samples A, C, and E of Fig. 2 are shown in Fig. 3.
In the case of 50% Sn-50% In target [Fig. 2(a)], the main
spectrum (Sn430 ) of Sn at 430 eV was stronger than the main
spectrum (In404 ) ofIn at 404 eV. In the case of the target with
a larger indium side [Fig. 2(b)] the line In404 was stronger
than Sn430 in contrast with first target. In each case, the
atomic concentration of Sn and In in ITO films was determined by measuring the peak-to-peak amplitude of the corresponding element (Sn 430 or In404 ) with elemental sensitivity factors,1O and was shown in Fig. 2. Due to the partial
overlap of Sn430 and In404 lines the accuracy of determination of concentrations is relatively low. An indirect indication of this accuracy may be drawn from the position of
resistivity minimum in Fig. 2(b). We think that this accuracy
is sufficient for the purpose of our semiqualitative analysis.
Our Auger data relate this minimum with approximately 1:9
ratio ofSn to In. A similar minimum found in 11 corresponds
to 4-6 wt. % of Sn02 in Sn:In 20 3 mixture.
It is obvious from Fig. 2 that the resistance correlates
with the relative concentration ofSn and In in the ITO film.

Position of Snlln target

Id~~~=T~lnC===~100
___........... In

Id

Con~i-.
I ""---.
I

Sn

80.-%

I
I

60Q

40ffi
()

I
I
I

a:

I-

20

1
A
B, CD
E
F
Ia) lO'---..;..t.;....--,----.J:-L.:L-....:L......i..--..IO

Posit ion of subs tr ate glass

3583

:5

25mm

~ 102 mm

J. Appl. Phys., Vol. 54, No.6, June 1983

80
FIG. 2. Room temperature sheet resistances of transparent conducting ITO
films with respect to the configuration of
Sn/In target and the position of substrate
glass. Electrodes length 5 mm, gap
between the two paralIel Au electrodes is
0.3 mm. (a) Symmetrical In/Sn target; (b)
nonsymmetrical In/Sn target. Insert to
Fig. 2(b): The configuration of the nonsymmetrical In/Sn target. 1-1-1: resistance; .-.-.: concentration.

~ld
z
~

(J)

ID
8 0::10

Sn

,0

10

In

~c.

'I

1'--__
"".~
Idl~_A~~B~_C~S~n_D~_E~-~F~~ o
Position of

(b)

substrate glass
M. Fujinaka and A. A. Berezin

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,:,e.

.~

C')

:d

1.0

;d

C')

:d

o::t

1.0

:d

C')

:d

1.0

:d

:0

In
Sn

430

In
404
(b)

In
404

The overall resistance of samples in Fig. 2(b) are higher than

those in Fig. 2(a) in spite of increasing the concentration of
In. The deposition rate was changed by increasing the area of
In target because In has a relatively lower sputtering rate. As
a result, under the same sputtering conditions (power, sputtering time, and constant flow rate: Ar: 100 cm3/min; O2 : 20
cm 3/min), the thickness of ITO film is smaller in the case of
In> Sn target than for the case when 50% Sn-50% In target
was used.
The relative concentration of oxygen in the ITO films
was constant regardless of the position of the substrate as
follows from almost constant Auger signal (0 520, about
50%). As a result, we can describe our ITO films as a variable composition mixture of Sn02 + x and In203+y (lxi,
Iyl <1), where x and y reflect the excess or deficit of a lattice
3584

J. Appl. Phys., Vol. 54, No.6, June 1983

In
404

oxygen relatively to the ideal stoichiometry. Sn02 was a

dominant participant when the symmetrical SnlIn target
was used [Fig. 2(a)], whereas In 20 3 dominated in ITO films
when the second, In-dominated target was used [Fig. 2(b)].
Then, we observed the spectral dependence of the optical transmittance in the visible region which is shown in Fig.
4(a) for the case of Fig. 2(a) target. The case of Fig. 2(b) target
is shown in Fig. 4(b). The relative transmittance of In-richer
ITO films was 80%-90% and rather spectrally unsensitive
in the visible region. At the same time the transmittance of
Sn-richer areas could be substantially imprOVed at a shorter
wavelength by increasing In concentration. The samples E
and F in Fig. 4(a) have spectral characteristics similar to
those shown in Fig. 4(b) due to the increasing proportion of
In as could be seen in the Auger signal.
M. Fujinaka and A. A. Berezin

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100

100

80

F........:.. -.-... - ~.:;;a-~

..........
",.,. .............(:4'~ ...-.
/E
/"%.".,.; ............

...

---

~60

~C

~
Z

80

.",eh./AI'
~,

. . . !/~
.......:.,&.,

FIG. 4. Optical transmittance for ITO films.

(a) For the target of Fig. 2(a); (b) for the target of Fig. 2(b).

t::

~40

C/)

...

--. .'_.,.
ABC

...-...

I-

..... - ..................
0

20

O~------~------~----~

0.4
la)

0.5

0.6

WAVELENGTH

0.7

(,u. m)

OL-------~------~-----~

0.4

0.5

IV. Cu 20 PREPARATION AND CHARACTERIZATION

We studied thin films of Cu 20 deposited by rf sputtering in constant Ar flow (flow rate 100 cm 3 /min) and various
Oz flow rates (5, 10,20,30, and 50 cm 3 /min) on glass. The Cu
target used for sputtering had 99.9% purity and was 3 mm in
thickness. All Cu2 0 films for the electrical conductivity
measurements were made by supplying an rf power level of
150 W for 20 min, and the films obtained had a thickness of
the order of 4500 A. Thickness of all CUzO films were measured by a Taylor-Hobson (TALYSURF4) probe.
Gold electrodes were evaporated on top of CUzO films
as shown in Fig. 5. The electrical conductivity of the films
was measured at room temperature and the results are also
shown in Fig. 5.
The obtained CUzO films exhibited a minimum in conductivity (0'min - 10- 3 n -1 cm - 1) at an oxygen flow rate of
approximately 20% that of Ar (100 cm 3 /min). The film
which corresponds to this ratio of flow rates probably corresponds to an ideal stoichiometry of CUzO. At lower Oz percentage than this minimum point, the conductivity of the
films increases because of the larger copper content than in
ideal CUzO. Higher levels of O 2 flow result in an increase of
the conductivity presumably because of the admixture of
CuO to CUzO. We also measured the thermostimulated conductivity of films fabricated at various Oz flow rates (10%,
20%, 30%, and 50% of Ar flow rate) in the region from
- 50C to + 85 C. The results are shown in Fig. 6. The
conductivity at a relative Oz flow rate of 5% is not shown
because the obtained film behaves like metallic Cu. The activation energy of the thermostimulated current of the films
corresponding to the oxygen flow rate of20% was calculated
from linear log I vs T - 1 plot (labeled in Fig. 6 as "Ozo"), and
is equal to 0.55 eV [assuming the conductivity -exp( - activation energy/2kT)].
Based on these results we have chosen the Oz and Ar
flow rates of20 cm3 /min and 100 cm 3 /min, respectively, for
the subsequent fabrication of CUzO photocells.
3585

J. Appl. Phys., Vol. 54, No.6, June 1983

0.6

WAVELENGTH

0.7

C)L m)

(b)

V. PROPERTIES OF ITO/Cu20 HETEROJUNCTION

CELLS

To produce an ohmic electrode for the cells, gold was

evaporated on the top of the CUzO films (20% Oz flow rate),
10

~~~~i!llZiI~r!H+--thin film

-5

10

-6

5X10

ro 10) 20 30 40 50
I

02 to Ar (%)

FIG. 5. Electric current for the films ofCu 2 0 deposited for various O 2 to Ar
flow ratios, at rf power level 150 W for 20 min, at bias of 5 V.
M. Fujinaka and A. A. Berezin

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200

250

T (K)

300

350 400

FIG. 7.1- V characteristics for the ITO/Cu,O/ Au cells at different sputtering power levels. The substrate is the ITO film at the position C in Fig. 2(a).

FIG. 6. Electric current vs reciprocal temperature for Cu 2 0 films of Fig. 5.

10, 020'
30, and 0'0 are 10, 20, 30, and 50% of 0, in the gas mixture,
respectively. Bias is 5 V.

which are deposited on glass coated with ITO films of different composition. Hence the resulting structure of the photocell could be specified as ITOICuzOI Au as illustrated in the
insert to Fig. 8.
In the case when the sputtering power level was 150 W,
we could not obtain samples having a rectifying 1- V characteristics, possibly because of the presence of many recombination centers at the junction interface of ITOICuzO formed
due to the particle bombardment during the discharge.
However, by decreasing the sputtering power level, we could
observe the characteristics such as shown in Fig. 7. The ITO
film used for the samples represented in Fig. 7 was a substrate of the type C from Fig. 2(a). For CUzO films sputtered
at a power level of75 W rectification can be obtained for all
types of composition of ITO films (i.e., A-F from Fig. 2).
The 1-V characteristics for the cells were measured under dark conditions and under illumination of about 100
mW cm- 2 (calibrated by light meter LI-I85A of LAMBDA
Instruments Corporation) with an incandescent lamp (Sylvania Co.) of 750 W placed 20 em from the face of the ITO
films. For the ITO films from Fig. 2(a), we were able to find
the dependence of the photo-output on the composition of
ITO films, but we could not find such pronounced depen3586

J. AppL Phys., Vol. 54, No.6, June 1983

rf power level (W)

thickness (A)

sputtering time (min.)

150

4500
2500

20

100
75

2000

30

25

dence when the ITO films from Fig. 2(b) were used. This
difference may be related with the overall high resistivity of
ITO films from Fig. 2(b) to that from Fig. 2(a) and with possible differences in conduction mechanisms of In z0 3 :Sn and
Sn02 :In films which are not yet fully understood. II
For the cells of the type A and F from Fig. 2(a), we did
not show their characteristics in Fig. 8, because of the possible influence of the end effects from the sputtering Cu target
and also because of the decrease of the photo-output.
PhotovoItaic output was studied only for ITO films of
the composition with Sn > In and the maximum open circuit
voltage was obtained for the ratio of Sn:In~85: 15.
For the cells deposited on substrates of the types B, C,
D, and E, the spectral distribution of output open circuit
60

lighti>

Au(2.5m rtI
cu 0
dia.)
2

ITO

substrate glass
-0.2

-0.1

0.2
V (v)

FIG. 8. Dark (solid lines) and iIluminated (dotted lines) I-V characteristics
for the cells fabricated on ITO substrates of different composition in Fig.
2(a). rf power level used: 75 W; sputtering time: 30 min; thickness of film:
2000 A.
M. Fujinaka and A. A. Serezin

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mW cm- z. The open-circuit voltage and the short-circuit

2
current were in the region 20 - 90 m V and about 50 /-LA/ cm ,
respectively, which is unfortunately insufficient for practical
solar cells.

1.0

For our data we estimated the standard photovoltaic

conversion parameters (see, e.g., 5 of Ref. 3). For the illuminated curve labeled as "B,C" in Fig. 8 we obtained

w
rJ)

00.5
Cl.

Voc =90 mY; jsc

........- ......... .........
/
'.
/0
. --_....... '."-.

rJ)

a:

~:I:

.......

Cl.

.",..

.'" E

q,:4

0.5

FF~O.27;

.-.

.--.~....

0.6

WAVELENGTH

.7

CJL m)

FIG. 9. Spectral distributions for the cells (of Fig. 8) made from ITO films of
Fig.2(a).

voltage was measured as the function of the wavelength as

shown in Fig. 9. The maximum photovoltaic peaks were essentially similar to those found for Cu/Cu 20 heterojunction
solar cells 4 or MIS-type CU/CU 2 0 cells. 6
VI. DISCUSSION AND CONCLUSIONS

The output characteristics for the ITO/Cu 2 0 photocells depended on the composition of both the ITO film and
the Cu 20 film.
The CuzO cells deposited by sputtering on the ITO
films ofB and C type (Sn:In=85: 15) exhibit I-V characteristics as shown in Fig. 8, and the polarity of photovoltage is
always positive on the gold contact side. The activation energy of 0.55 eV for CuzO film was found from thermostimulated conductivity whereas the band gap of 2.0 eV was found
from the spectral dependence of the photovoltaic effect.
Therefore, we can propose a barrier band diagram for ITO/
CuzO cells such as shown in Fig. 10.
The photovoltaic characteristics of ITO/Cu 2 0 cells
were measured under an incandescent lamp with 100
ITO

Au

FIG. 10. Energy band diagram for ITO/Cu,O cells.

3587

45/-LA/cm2,

Vmp =48 mY; jmp=23/-LA/cm 2 ,

.,,,.
........

.",,-

J. Appl. Phys .. Vol. 54. No.6. June 1983

77=10- 3 %.

This undoubtedly very low value of the conversion efficiency of CU20/ITO for our thin film photocell does not,
however, finally discard the Cu 20 as a feasible photovoltaic
material. For single crystal Cu 20/Cu Schottky barrier photocells conversion efficiencies of = 1% have been demonstrated under AMI illumination. 7 Even higher values of 77
(up to 3%) were obtained for a monochromatic illumination
(A~675 mm, illumination level ~60 /-L W /cm 2 ) in our previous study?
The study2 was carried out on single crystal Cu20/Cu
photocells. At the same time, the study of thin films CuzO/
Sn02 cells prepared by electrodeposition 8 again resulted in
very low values of Voc andjsc (V ~50 m V andjsc =50 /-LA/
cm 2 for AMI conditions) comparable with our present values. These results allow us to suggest that low conversion
efficiencies of thin films Cu 20 cells are related with deficiencies of the presently used thin film techniques for Cu 2 0,
rather than with the cuprous oxide itself. The chief problem
here is, in our opinion, the high resistivity of deposited Cu 2 0
films (which limits jsc) rather than limitations related with
the low barrier height.
At the same time, we have to note that our Cu 20 films
show the typical x-ray diffraction pattern of amorphous material (see Fig. 11), and probably have a high concentration of
recombination centers in the interfacial layer (these centers
may be related with trace impurities in ITO) which tends to
lower the barrier height of the junction. These two reasons
are likely to have a detrimental effect of the photovoltaic
output characteristics.
In this connection we should mention that attempts
have been made to explain the "efficiency plateau" of Cu 20
cells on the basis of poor barrier quality. 9 In this respect, the
special study of diffusion lengths in Cu 20 thin films may
provide a better insight into the future prospectives of cuprous solar cells.
Figure 11(a) shows the x-ray diffraction pattern for a
Cu 2 0 film of 5500-A thickness deposited during sputtering
at an rf power level of 150 W for 30 min.
For comparison, in Fig. 11(b) we show the diffraction
pattern (Cu KaJ line; A = 1.54 A) of CuzO powder prepared
chemically. In contrast with a thin film pattern [Fig. l1(a)]
this pattern shows a more pronounced crystalline structure.
From Fig. 11 (b) we determined the Miller index (1.1.1) at the
Interplanar spacing of d = 2.46 A assuming the cubic structure.
In this study, the oxygen flow was kept constant during
the fabrication of ITO films. The amounts of oxygen during
DC

M. Fujinaka and A. A. Sarazin

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------.--- r--

,...

FIG. II. X-ray diffraction patterns; (a) for

the Cu 2 0 film of5500 Athickness deposited by supplying rf power level of 150 W for
30 min; (b) for the powder of Cu,O made
chemically.

46

44

42

40

38

the deposition as well as during the heat annealing after deposition are important for the improving of the photovoltaic
output, since electrical resistance is affected strongly by both
of them. So, in terms of preparation characteristics, the low
efficiencies of our cells can be reasoned by insufficient optimization of oxygen flow parameters. As illustrated by Figs. 5
and 6, the Oz to Ar ratio has a very pronounced effect on the
conductivity of ITO and CUzO films.
In conclusion, we can stress that the height of the potential barrier at junction interface is strongly influenced by the
amount of available oxygen during the various stages of the
fabrication process.
One can also tentatively attribute the very low conversion efficiencies observed for thin films Cu 2 0/ITO cells to
either small diffusion length or to interface recombination
centers. Both these reasons can also act jointly and eventually could be related to the above-mentioned excessive or deficient oxygen.
Keeping in mind the fact that both thin film components of our cells (Cu 2 0 and ITO) were produced by the same
rf sputtering process, the system Cu 2 0/ITO could be interesting from the viewpoint of mass production, provided the
photo voltaic output could be substantially increased by the
proper control of the preparation conditions. As one of the
probable ways to increase the conversion efficiency, we can
mention here the temperature annealing of ITO films as well
as the use of higher purity starting materials.

3588

J. Appl. Phys., Vol. 54. No.6, June 1983

ACKNOWLEDGMENTS

This work was supported by the Natural Sciences and

Engineering Research Council of Canada. The authors also
thank N. Dalacu for technical assistance on thin film preparation and B. Diacon for help during the measurement of
Auger characteristics.

1M. Fujinaka and A. A. Berezin, Thin Solid Films 101,7 (1983).

2A. A. Berezin and F. L. Weichman, Solid State Commun. 37,157 (1981).
JA. A. Berezin and F. L. Weichman, Phys. Status Solidi A 71,265 (1982).
4J. Herion, E. A. Niekisch, and G. Scharl, 14th IEEE Photovoltaic Spec.
Conference, San Diego, California 1980 (IEEE, New York, 1980), p. 453.
'L. Papadimitriou, N. A. Economou, and D. Trivich, Sol. Cells, 3, 73
(1981).
6L. C. Olsen, F. W. Addis, and R. C. Bohara, 14th IEEE Photovoltaic Spec.
Conference, San Diego, California, 1980 (IEEE, New York, 1980), p. 462.
7D. Trivich, E. Y. Wang, R. J. Komp, and A. S. Kahar, 13th IEEE Photovoltaic Spec. Conference Washington, D. c., 1978 (IEEE. New York,
1978), p. 174.
"N. A. Economou, R. S. Toth, R. J. Komp, and D. Trivich, in Photovoltaic
Solar Energy Conference, Luxembourg, 1977 (Reidel-Dordrecht, Boston,
1978), p. 1180.
"L. C. Olsen, R. C. Bohara, and M. W. Urie, Appl. Phys. Lett. 34, 47 (1979).
IOL. E. Davis, N. C. MacDonald, P. W. Palmberg, G. E. Riach, and R. E.
Weber, Handbook of Auger Electron Spectroscopy (physical Electronics
Industries, Minnesota, 1976).
11M. Mizuhashi, Thin Solid Films 70,91 (1980).

M. Fujinaka and A. A. Serezin

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