Photoluminescence characterization of Al/Al₂O₃/InP MIS structures passivated by anodic oxidation
Metal-insulator-semiconductor (MIS) structures were produced by electron beam heating evaporation of Al₂O₃ on InP. Polyphosphate thin films with the thickness of 100 to 150 A were used to passivate the interface InP/Insulator. Photoluminescence spectra were obtained at low temperatures at the variou...
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Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
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irk-123456789-1192292017-06-06T03:04:05Z Photoluminescence characterization of Al/Al₂O₃/InP MIS structures passivated by anodic oxidation Mahdjoub, A. Bouredoucen, H. Djelloul, A. Metal-insulator-semiconductor (MIS) structures were produced by electron beam heating evaporation of Al₂O₃ on InP. Polyphosphate thin films with the thickness of 100 to 150 A were used to passivate the interface InP/Insulator. Photoluminescence spectra were obtained at low temperatures at the various stages of MIS-InP structure formation. At ambient temperature, photoluminescence topography made it possible to characterize the surface state after each technological stage. The interface degradation under the effect of repeated annealing is insignificant up to the temperatures close to 350 °C. Major radiative defects detected using photoluminescence spectrum with energies ranged from 0.95 to 1.15 eV were attributed to the impurity complexes of phosphorus vacancies, concentration of which is substantially reduced in the presence of anodic oxide. 2004 Article Photoluminescence characterization of Al/Al₂O₃/InP MIS structures passivated by anodic oxidation / A. Mahdjoub, H. Bouredoucen, A. Djelloul // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2004. — Т. 7, № 4. — С. 436-440. — Бібліогр.: 16 назв. — англ. 1560-8034 PACS: 42.79.Wc, 78.20.-e, 71.55.Eq, 73.20.-r, 78.55.-m http://dspace.nbuv.gov.ua/handle/123456789/119229 en Semiconductor Physics Quantum Electronics & Optoelectronics Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
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Metal-insulator-semiconductor (MIS) structures were produced by electron beam heating evaporation of Al₂O₃ on InP. Polyphosphate thin films with the thickness of 100 to 150 A were used to passivate the interface InP/Insulator. Photoluminescence spectra were obtained at low temperatures at the various stages of MIS-InP structure formation. At ambient temperature, photoluminescence topography made it possible to characterize the surface state after each technological stage. The interface degradation under the effect of repeated annealing is insignificant up to the temperatures close to 350 °C. Major radiative defects detected using photoluminescence spectrum with energies ranged from 0.95 to 1.15 eV were attributed to the impurity complexes of phosphorus vacancies, concentration of which is substantially reduced in the presence of
anodic oxide. |
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Mahdjoub, A. Bouredoucen, H. Djelloul, A. |
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Mahdjoub, A. Bouredoucen, H. Djelloul, A. Photoluminescence characterization of Al/Al₂O₃/InP MIS structures passivated by anodic oxidation Semiconductor Physics Quantum Electronics & Optoelectronics |
| author_facet |
Mahdjoub, A. Bouredoucen, H. Djelloul, A. |
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Mahdjoub, A. |
| title |
Photoluminescence characterization of Al/Al₂O₃/InP MIS structures passivated by anodic oxidation |
| title_short |
Photoluminescence characterization of Al/Al₂O₃/InP MIS structures passivated by anodic oxidation |
| title_full |
Photoluminescence characterization of Al/Al₂O₃/InP MIS structures passivated by anodic oxidation |
| title_fullStr |
Photoluminescence characterization of Al/Al₂O₃/InP MIS structures passivated by anodic oxidation |
| title_full_unstemmed |
Photoluminescence characterization of Al/Al₂O₃/InP MIS structures passivated by anodic oxidation |
| title_sort |
photoluminescence characterization of al/al₂o₃/inp mis structures passivated by anodic oxidation |
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Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
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2004 |
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http://dspace.nbuv.gov.ua/handle/123456789/119229 |
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Photoluminescence characterization of Al/Al₂O₃/InP MIS structures passivated by anodic oxidation / A. Mahdjoub, H. Bouredoucen, A. Djelloul // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2004. — Т. 7, № 4. — С. 436-440. — Бібліогр.: 16 назв. — англ. |
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Semiconductor Physics Quantum Electronics & Optoelectronics |
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AT mahdjouba photoluminescencecharacterizationofalal2o3inpmisstructurespassivatedbyanodicoxidation AT bouredoucenh photoluminescencecharacterizationofalal2o3inpmisstructurespassivatedbyanodicoxidation AT djelloula photoluminescencecharacterizationofalal2o3inpmisstructurespassivatedbyanodicoxidation |
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2025-07-08T15:28:41Z |
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Semiconductor Physics, Quantum Electronics & Optoelectronics. 2004. V. 7, N 4. P. 436-440.
© 2004, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
436
PACS: 42.79.Wc, 78.20.-e, 71.55.Eq, 73.20.-r, 78.55.-m
Photoluminescence characterization of Al/Al2O3/InP MIS structures
passivated by anodic oxidation
A. Mahdjoub1, H. Bouredoucen2, A. Djelloul1
1 Laboratoire des Matériaux, Structure des Systèmes
Electroniques et leur Fiabilité, Centre Universitaire d'Oum El Bouaghi, Algerie
2 Electrical and Computer Engineering Department, Sultan Qaboos University, Muscat, Oman
Abstract. Metal-insulator-semiconductor (MIS) structures were produced by electron
beam heating evaporation of Al2O3 on InP. Polyphosphate thin films with the thickness
of 100 to 150 Å were used to passivate the interface InP/Insulator. Photoluminescence
spectra were obtained at low temperatures at the various stages of MIS-InP structure
formation. At ambient temperature, photoluminescence topography made it possible to
characterize the surface state after each technological stage. The interface degradation
under the effect of repeated annealing is insignificant up to the temperatures close to
350 °C. Major radiative defects detected using photoluminescence spectrum with
energies ranged from 0.95 to 1.15 eV were attributed to the impurity complexes of
phosphorus vacancies, concentration of which is substantially reduced in the presence of
anodic oxide.
Keywords : indium phosphide, MIS structures, photoluminescence.
Manuscript received 28.10.04; accepted for publication 16.12.04.
1. Introduction
The performance advantages of the compound
semiconductor indium phosphide (InP) cannot be fully
exploited in microwave and optoelectronic systems until
a process is developed to control surface-related
instabilities and failure mechanisms. In spite of the
promising properties of InP, the problems which slow
down the expansion of MISFET-InP are still far to be
solved. The passivation of the surface of the III-V
compound is necessary. Various chemical treatments
were studied [1-4]. The electrochemical approach used
in several previous works [5-7] allows to better control
the treatment and a broad range of oxidation parameters,
which affect the properties of the obtained oxide.
However, in recent years, there have been many reports
on the potential passivating properties of anodic oxide
for the interface of the MIS-InP structures [8, 9]. The
characterization of the interface of the MIS structures is
generally based on measurements of high frequency
capacitance (Terman analysis) or on quasi-static mode
(Berglund technique). These methods require the use of
good quality dielectric material deposited by relatively
soft methods to preserve the fragile surface of InP [10].
Thus, it is interesting to develop new characterization
methods of the interface to overcome these constraints.
Of all the properties that characterize photoluminescence
(PL), the intensity of the PL signal has received the most
attention in the analysis of interfaces. This interest is due
to the fact that, although several important mechanisms
affect the PL response, it is generally found that large PL
signals correlate with good interface properties. PL is a
simple method, fast, contactless, nondestructive and
sensitive to the presence of interface defects [1, 10, 11].
Being a direct gap semiconductor, InP has a very high
measured PL signal even at room temperature. Broad
ranges of utilization can be made possible for this
characterization technique, namely: PL spectra at low
temperature, PL topography (PLT), integrated PL at
ambient temperature, and PL under electric polarization
[10-13]. If the setting of this characterization method can
be made simple and very flexible to use, the
interpretation of the measurements results are still
remaining very delicate. The differences in the PL
intensities observed are generally attributed to the
interface or surfaces defects and/or to the electric
potential of surface.
In this work, we present a simple and useful method
for preparing MIS structures on InP with a reduced
complexes impurities of phosphorus vacancies. In
addition, the objective is to track the changes of the PL
spectra as well as the changes in its topography
measured after various technological realization stages
of MIS on InP structures subjected to electrochemical
treatment.
2. Experiment
Two standard samples of (100) oriented n-InP doped
(~1016 cm–3) were used. Samples were cleaned in hot
Semiconductor Physics, Quantum Electronics & Optoelectronics. 2004. V. 7, N 4. P. 436-440.
© 2004, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
437
trichloroethylene and rinsed in methanol, and deionized
water. They were briefly etched in 40 % HF solution for
60 s to remove surface defects and oxide layers.
Immediately the reference PL spectrum as well as a PLT
are reported on one of these two samples. The second
sample undergoes an electrochemical treatment using the
solution of AGW composed of 3 % diluted
orthophosphoric acid (pH = 2) mixed in glycol
propylene in 1:2 ratio. Anodic oxidation of InP is carried
out under white light illumination. The first oxidation
phase is known as galvanostatic where the current
density remains 0.2 mA⋅cm–2 until the terminal voltage
of the oxidation cell reaches 20 V, and then the
potentiostatic mode switched to a softer termination of
the treatment. The double-layered structure is a typical
to this kind of oxide. The outer indium-rich thin layer
strongly hydrated exhibits poor dielectric properties. At
the interface, one finds a thicker layer of condensed
phosphates of better quality similar to In(PO3)3. The
outer layer is dissolved using 0.01 % diluted HF solution
for 120 s which allows keeping a phosphorus-rich layer
of 150 Å thickness. Then the sample undergoes
annealing at 250 °C in N2 atmosphere during 20 min to
eliminate any residual water traces. The following
technological step consists of depositing the insulator
(1000 Å of Al2O3) on these two samples. The deposition
is carried out by electron beam heating evaporation
within secondary vacuum environment and under
oxygen partial pressure. This technique is based on the
heat produced by high energy electron beam
bombardment of the material to be deposited. The
electron beam is generated by an electron gun, which
uses the thermoionic emission of electrons produced by
an incandescent filament (cathode). Emitted electrons
are accelerated towards an anode by a high difference of
potentials (kV). The crucible is perforated disc able to
act as the anode. A magnetic field is often applied to
bend the electron trajectory, allowing the electron gun to
be positioned below the evaporation line. An annealing
at 300 °C in oxygen atmosphere during 30 min allows to
compensate the deficiency of oxygen, which is generally
observed in this type of deposit. The final annealing in
forming gas (H2-N2) at 350 °C for two hours is
performed to cure certain interface defects and to
improve the quality of the structure. To finish the
fabrication of the MIS-InP structure, some
semitransparent aluminium contacts can be deposited for
PL measurements under electrical polarization.
Measurements of PL spectra and PLT were carried out
after every technological step and every annealing.
Liquid nitrogen photoluminescence data were collected
by Oriel 7240 monochromator with an argon laser at the
wavelength of 514.5 nm and output power of 100 mW.
The sample receives only 3 mW distributed on a spot of
2.2 nm in diameter. A silicon detector covers a spectral
field extending from 430 to 1060 nm. The PLT
measurements were performed in air at the room
temperature. The sample put on the X-Y plane was
moved under a focused laser beam in a such a manner
that the data of PLT measurements were obtained.
632.8 nm line of He-Ne laser (power 5 mW) was used
for excitation, and the spot diameter of the focused laser
beam was ranged from 3 to 80 µm. A silicon photodiode
was used to receive the excited PL signals. The device is
completely controlled by computer. A comparative study
of various measurements is made possible and allows
presenting conclusions as far as the influence of the
treatment used on the quality of the structure is
concerned.
3. Results and discussions
3.1. Photoluminescence
The reference spectrum obtained on uncovered substrate
is typical for an n-InP sample [14-16]. It presents three
essential typical peaks as shown in Fig. 1. The highest
peak I1 located at 1.41 eV shows a luminescence close to
the gap, which is due to bound excitons related to the
surface impurities. The broader peak I2 located at
1.37 eV is attributed to the band-acceptor or donor-
acceptor transitions. The broader band I3 having the
energy in the interval ranged from 0.95 to 1.15 eV also
known as the “band C” is generally attributed to the
impurities (Fe, Cu, Mn, Co, Zn) forming complex
defects with the phosphorus vacancies.
A qualitative indication of passivation is therefore
achieved by comparing the PL intensity of the HF pilot
sample passivated InP surface with that unpassivated InP
surface. Table 1 shows the PL results for the InP surface
measured at 77 K according to the conditions of the
subsequent processing. The PL spectra obtained after
anodic oxidation and dry annealing presents a
comparable shape to proceeding with a considerable
reduction of the intensities of all peaks. However, an
increase in I1/I2 ratio is noticable. This behavior can be
attributed to a strong curving the energy bands close to
the surface due to negative charges existing in the
condensed anodic phosphates In(POx)y. Indeed, y is
generally higher than 3, corresponding to the
stoichiometry. In addition to this, the measurements of
the capacitance-voltage (C-V) characteristics on thicker
anodic oxides (around 800 Å) has shown an apparent
shift towards positive voltages, which indicates a
situation of depletion at the rest. However, this
observation does not completely exclude the presence of
defects in InP-oxide interface involving nonradiative
recombination. After deposition of the insulator onto
these two samples, we can clearly notice (see Table 1)
the difference between a surface protected by the anodic
oxide and an uncovered InP surface. The PL increased
considerably for the electrochemically treated sample,
then it strongly decreased for the untreated sample. It is
clear that the deposition of Al2O3 by evaporation using
the electron gun considerably degrades the fragile
surface of InP. The increase of luminescence from the
Semiconductor Physics, Quantum Electronics & Optoelectronics. 2004. V. 7, N 4. P. 436-440.
© 2004, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
438
Table 1. PL results of the InP surface measured at 77 K according to the conditions of the subsequent processing.
Second annealing
First treatment Al2O3 deposition
First annealing O2-
30 min (H2-N2)- 2 h
PL
intensity Sample HF
Anodic
oxidation
Sample
HF
Anodic
oxidation Sample HF
Anodic
oxidation
Sample
HF
Anodic
oxidation
I1 (%) 100 31 22.4 168 20.5 65.9 25.8 57.4
I2 (%) 28 4.6 3.5 23.5 3.4 5.7 4.4 4.2
I3 (%) 13 4.8 3.8 4.5 34.2 7.5 274.7 9.1
I1/I2 3.6 6.7 6.4 7.1 6.0 11.6 5.9 13.7
I1/I3 7.7 6.5 5.9 37.3 0.6 8.8 0.1 6.3
Table 2. Integrated photoluminescence measured at 300 K after each technological step.
Samples Initial еreatment
Deposition of Al2O3
and annealing O2 Annealing H2-N2
Standard HF 100 % 5 to 10 % < 5%
InP/ anodic
oxide 10 to 20 % 30 to 40 % 25 to 30 %
Fig. 1. PL spectra of InP surface measured at 77 K after
annealing in oxygen ambient at 300 °C: (a) HF pilot sample;
(b) passivated InP surface; (c) unpassivated InP surface.
Fig. 2. PL spectra of InP surface measured at 77 K after
annealing in forming gas (H2-N2) at 350 °C: (a) HF pilot
sample; (b) passivated InP surface; (c) unpassivated InP
surface.
treated sample can only be explained by a change in the
potential of surface due to a total positive charge in the
deposited Al2O3. This positive charge is caused by the
oxygen deficiency generally reported for this type of
deposits. An annealing in oxygen atmosphere is
generally necessary to improve the quality of Al2O3
deposited in this way [9]. After annealing in oxygen at
300 °C for 30 min, Al2O3 loses its positive charge while
approaching the stoichiometry which once reached
modifies curving the energy band at the interface. The
intensity of the peak I1 (Fig. 1) decreases but remains
relatively high (66 % of reference I1) compared with that
of the pilot sample (20 %). For the sample treated, the
ratio I1/I3 is comparable with that of the reference
spectrum (Table 1); thus, the surface is well preserved
during the deposit process. Thermal annealing is
generally used in the technological process to cure the
interface defects caused by the insulator deposit. An
annealing at 350 °C in forming gas (H2-N2) during two
hours is recommended [9]. The PL spectra obtained for
these two samples having undergone the same annealing
are presented in Fig. 2. We can clearly notice the
profound effect of electrochemical treatment on the
surface of InP. The ratio I1/I3 is by the order of 6 for the
protected surface (its value for the reference sample lies
between 7 and 8) and only 0.1 for nonprotected samples.
The increase of the peak I3 after annealing at high
temperatures is generally attributed to the phosphorus
vacancies and/or the complex defects combining
impurities and vacancies [14-16]. To explain the
important role of anodic oxide, one can evoke the
following two arguments:
Semiconductor Physics, Quantum Electronics & Optoelectronics. 2004. V. 7, N 4. P. 436-440.
© 2004, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
439
Fig. 3. PL images measured at 300 K: (a) pilot sample etched in 40 % HF for 60 s, IPL=100 %; (b) passivated InP surface after
deposition of Al2O3 and annealing in oxygen at 300 °C for 30 min, IPL = 30…40 %; (c) InP surface anodically oxidized and
annealed in nitrogen for 30 min at 200 °C, IPL = 10…20 %; (d) uncovered InP after deposition of Al2O3 and annealed in oxygen at
300 °C for 30 min, IPL = 5…10 %.
a) the condensed polyphosphates which are rich
with phosphorus create a diffusion barrier and
prevent the decomposition of InP on exposure to
temperatures;
b) the protected surface during deposition is less
damaged, and hence, it is becoming less
vulnerable to the effect of repeated annealing.
3.2. Photoluminescence mappings
Because PL intensity is an indicator of interface
quality, the measurements of the PL signal vs position
provide information on the spatial uniformity of
interface properties. Fig. 3 shows some PLT taken on
1×1 mm2 surface located on targeted regions at the
surface of these two samples. Table 2 shows the
average values of integrated PL measured at 300 K on
these two samples after each technological step. The
PL is standardized and compared to the reference
signal reported on the uncovered InP. It is generally
admitted that a high PL signal is an indication of a
good quality of the interface [14]. This fact confirms
once again the dominant role of the electrochemical
treatment on the Al2O3/InP interface. For the
protected sample, about 30 % of the PL signal is
preserved, whereas for the non-protected surface, the
PL signal decreases to 10 % after Al2O3 deposition
and becomes less than 5 % after two thermal
annealing. The surface of the treated sample is more
homogeneous, because the anodic oxidation moves
the interface towards the volume of the substrate and
thus eliminates many surface defects (buried surface).
In the end of study, we have proceeded to the
scouring of the deposited Al2O3 on these two samples.
Electrochemically treated surface is relatively
preserved, whereas the untreated InP surface is
characterized by a coloured white-silver which
testifies to the presence of the indium metal at the
surface and thus an irreversible decomposition of InP
at high temperatures.
Semiconductor Physics, Quantum Electronics & Optoelectronics. 2004. V. 7, N 4. P. 436-440.
© 2004, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
440
4. Conclusion
The results obtained by our spectroscopic measurements
of PL and PLT confirm the profound effect of the
condensed polyphosphates In(POx)y on the interface
quality of MIS-InP structures. Electrochemical oxidation
allows moving the interface towards the volume and thus
eliminates many surface defects. It highly improves the
homogeneity and the quality of the samples. The anodic
oxide protects the fragile InP substrate during the
deposition of Al2O3. The phosphorus-rich condensed
phosphates obtained by electrochemical deposition from
a diffusion barrier and limit the creation of phosphorus
vacancies as well as their complex defects during
various annealing. We are expecting that the PL
measurements under electrical polarization will allow
the determination of surface states density. In addition,
to the above, other different chemical treatments will be
considered in the future and the previous assessing
techniques used.
Acknowledgements
We would like to thank the research groups of Prof. J.
Joseph and Prof. S.K. Krawczyk of ECLyon for their
assistance in accomplishing this work.
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Semiconductor Physics, Quantum Electronics & Optoelectronics. 2004. V. 7, N 4. P. 436-440.
© 2004, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
441
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