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Heat treatment effect on p type Zn doped InP substrates
A. Dhouib, B. Maloumbi, C. Martinez, L. Gouskov, D. Bayaa, T. Bretagnon, R. Coquille
To cite this version:
A. Dhouib, B. Maloumbi, C. Martinez, L. Gouskov, D. Bayaa, et al.. Heat treatment effect on p type
Zn doped InP substrates. Revue de Physique Appliquée, Société française de physique / EDP, 1987,
22 (10), pp.1159-1168. �10.1051/rphysap:0198700220100115900�. �jpa-00245664�
1159
Heat treatment effect
onp type Zn doped InP substrates
A.
Dhouib,
B.Maloumbi,
C. Martinez(*),
L.Gouskov,
D.Bayaa (1),
T.Bretagnon (1)
and R.
Coquillé (2)
Centre
d’Electronique
de Montpellier(CEM)
associé au CNRS(USA 391),
Université des Sciences etTechniques
du Languedoc, place E. Bataillon, 34060Montpellier
Cedex, France(1) Groupe
d’Etudes des Semi-conducteurs(GES)
associé au CNRS, Université des Sciences etTechniques
duLanguedoc, p1.
E. Bataillon, 34060Montpellier
Cedex, France(2)
Centre National d’Etudes des Télécommunications(CNET),
route de Trégastel, BP 40, 22301 LannionCedex,
France
(Reçu
le 15septembre
1986, révisé le 2 mars 1987, accepté le 5 juin1987)
Résumé. 2014 Au cours du processus d’élaboration de
photodiodes
InP n+/p
pour la conversion d’énergie solairepar diffusion de soufre à 700 C dans des substrats d’InP
dopés
Zn, lespropriétés électriques
etphotoélectriques
des substrats sont fortement modifiées. Les mêmes effets sont observés après unsimple
recuitdes substrats à la même température. La modification la plus notable est une forte augmentation de la densité de trous
(plus
d’un ordre degrandeur)
uniforme enprofondeur.
Unedégradation superficielle
des paramètresphotoélectriques, longueur
de diffusion L et durée de vie 03C4 des porteurs a aussi été observée. Lespièges profonds
détectés dans les substrats après traitementthermique
ne sont pastypiques
de ce traitement.Abstract. 2014
During
the process of elaboration of n+/p
InPphotodiodes
for solar energy conversion, we haveobserved that the 700 C sulfur diffusion into Zn
doped
InP substratesstrongly
modifies the electrical andphotoelectrical properties
of these substrates. Asimple annealing
at the same temperature produces nearlyequivalent
effects. The most relevant modification is a strong,depth independent
holedensity
increase(more
than one order of
magnitude).
Adegradation
of thephotoelectrical
parameters : diffusionlength
L and carrier lifetime 03C4 has also been detected near the surface of the heat treated substrates. Thedeep
traps measured fromdeep
level transient spectroscopy(DLTS)
are nottypical
of the heat treatment.Revue Phys.
Appl.
22(1987)
1159-1168 OCTOBRE 1987, PAGEClassification
Physics
Abstracts8140G - 8140R
1. Introduction.
InP has received
increasing
attention in the past few years because it is an attractive material forhigh speed circuits,
infrared(IR) photodetection
andsolar cells.
Very
efficient devices havealready
beenrealized in these
investigation
fields[1-3]. Among
the various steps involved in device
processing,
heattreatments are
required
for contactformation,
im-purity diffusion, implantation annealing.
The III-Vcompounds
are very sensitive to these heat treat- ments which maystrongly modify
notonly
thesurface
properties
but also the characteristics of the bulkstarting
material. Aninvestigation
of the heattreatment effects is therefore necessary in order to obtain a better control of the process parameters.
During
the elaboration of n+/p
InPphotodiodes
for solar energy conversion
by
sulfur diffusion at700 C into Zn
doped
p type substrates we have observed a strong modification of thedoping
levelinto the substrate. This paper describes this effect.
In order to check the influence of sulfur on this
modification,
the substrates have also been submit- ted tosimple
700 Cannealing
processes.In
InP,
Zn is acommonly
used p typedopant
andsome
investigators
havealready
noticed that such substrates were affectedby
heat treatments[4-5]
giving
rise todoping
level modification and trapsintroduction ;
the modelsthey
haveproposed
toexplain
these modifications will becompared
to ourresults.
Besides the main effect of hole
density
increase,we have also measured the
photoelectrical
par-Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/rphysap:0198700220100115900
ameters
(diffusion length
and carrierlifetime)
andthe traps into the heat treated substrates.
2.
Experimental.
The
investigated samples
were p type Zndoped
LEC grown InP
crystals.
Thecrystals
50 and 158come from CNET
(*),
thecrystal
148 wasprovided by Crystacom.
2.1 HEAT TREATMENTS. - Heat treatments were
performed
at 700 C in a sealedquartz ampoule. A phosphorus
overpressure was insuredby,
a red Pcharge
or InPpowder.
Thistype
of treatment is very similar to thermalimplantation annealing
condition.As
explained
in the introduction twotypes
of heat treatedsamples
have beeninvestigated :
- annealed
samples (only
Pcharge
in the am-poule)
- sulfur diffused
n+ /p samples ;
in this case,In2S3
was added to the Pcharge (In2S3 -
1 mg ; P : 1.5 mg is the 5cm3 ampoule).
The time of heat treatment : t was varied between 1/2 h and 90 h.
2.2 INVESTIGATION METHODS. - In order to inves-
tigate
the substratemodifications,
various characteri-zations have been made :
- Hall effect measurements
(Van
der Pauwmethod)
before and after the heattreatment
withand without sulfur diffusion.. .
-
Electrical
andphotoelectrical
measurementson
n+ /p
sulfur diffusedjunctions
and on semi-transparent
Au/InPSchottky
diodes.-
Deep
level transient spectroscopy(DLTS)
measurements.
The annealed
samples
will be identifiedby
thereference number of the substrate followed
by
theletter T in the case of
simple
heat treatment and S inthe case of sulfur diffusion. The as-grown substrate will be denoted A. The
Schottky
diodes have been made at variousdepths
into the heat treated sub- strate,they
are noted Sch 0(on
thesurface)
Sch 1(1 >m deep),
Sch 3(3 >m deep),
Sch 10(10 03BCm deep).
3. Results and discussion.
3.1 FREE HOLE DENSITY VARIATION. - The com-
parison
of the hole carrierdensity
andmobility
values before and after treatments is
given
in table I.Figure
1 presents the variations of the holedensity (p =1/RH q, RH :
Hallconstant)
versus103/T
measured on
samples
50A,
50T,
148A,
148 T.Table I. - Electrical characterized
of
various Zndoped
InP substrates submitted to 700 C heat treatments - p :(cm-3)-Jlp : (cm2fV.s).
CNET : Centre National d’Etude des Télécommunications, France.
1161
Fig.
1.- - 1
as a function of103 T
for thesamples
50 A, 50 T, 148 A, 148 T. Heat treatment time t = 12 h.
- The most relevant effect observed on heat treated
samples
for any heat treatment time is thestrong
p increase(greater
than one order of mag-nitude).
Hole densities deduced from Hall measure- ments on the as-heat-treated substrates and after acontroled
etching
of some tenths of microns of thesame substrates are
identical, showing
that the holedensity
is uniform into the substrate.The hole
density
increase varies between some1014
and1016 cm- 3
for the lessdoped crystal ;
3 to9 x
1016 cm- 3
for thecrystal
50(original density :
1.1 x
1015 cm- 3) ;
3 x1016 cm- 3
for thecrystal
158(original density :
1.8 x10 17 cm- 3).
- C-V measurements on
Schottky
diodes or Sdiffused
junctions
confirm the holeincrease ;
the C-V densities exhibit some weaker values than
1/RH q ,
Jvalues, they
are similar onSchottky
diodes Sch0,
3and 10.
- Before heat treatment, Hall effect measure-
ments on various
samples
of thecrystal
148 havedemonstrated a
good homogeneity
of thisstrongly compensated crystal.
After heat treatment, hole densities at 300 K vary from1014 cm- 3
to 1.6 x1016 cm- 3.
The C-V measurements ofSchottky
diodes made on this resistive substrate have been made at low
frequency (103-104 Hz).
A discussion of these electrical results can be made
taking
into account twocomplementary
infor-mations.
a)
SIMSprofiles
of Zn have been madeby
H.Gauneau on the substrate 50
[6]
and on the substrate 148.They
are ffat and identical before and after heat treatment :Nzn
= 7 x1016 cm- 3 (crystal 50), Nzn =1016 cm-’ (crystal 148).
b)
The Zn acceptor activation energy has been deduced fromphotoluminescence
measurements.Ea
= 47 meV inagreement
with the determination of E. Kubota[7]
and E. W. Williams[8].
Nodeeper
level appears after heat treatment.
- Model
of
Zn outdi f fu,sion.
- A Zn out-diffusion model has been
proposed by
CCDWong [5]
to describe the heat treatment effect on Zndoped
InP
crystals
on the as grown substrate : Zn atoms arepresent
in the lattice as substitionalacceptor Zns
and interstitialcompensating
donorZni ; during
heat treatment, the
Zn.,
atoms remainunchanged
whereas the
Zni
suffer an out-diffusion and evapo-rate at the surface
leading
to a decrease of compen- sation. CCDWong
based his model on the exper- imental observations of a Zn loss into the heat treated substrates(SIMS measurements)
and on theexistence of a carrier concentration
profile (deduced
from electrical
measurements).
This model
desagrees
with our results because :1)
Thepredicted
decrease of Zn atoms has notbeen observed in our SIMS measurements.
2)
Thepredicted inhomogeneous ,
hole densitiesinto the
substrate,
for moderate treatment times at700 C,
have not been observed in electricalmeasurements.
- Model
of
Zn activation. - Thedensity
of Znatoms
being unchanged
after heat treatment, it can bethought
that the increase of carriersmight
be dueto an electrical activation of Zn : interstitial Zn
(Zni) turning
substitutional Zn(Zn,,).
In order to check this
hypothesis,
the Hall effectmeasurements have been
compared
to the holedensity
deduced from the relation :valid in the case of a
compensated
p type semicon- ductor :Na is
the acceptordensity : Na
=NZns
if Znis the
only
acceptor.Na
is the donordensity : Nd
=Nzi
+Ndr ;
the residual donorsNdr
into InPare
generally
sulfur and silicon. SIMSprofiles
meas-urements have been made on the
crystal
50 beforeand after heat treatment, the sulfur
density (5
x1015
cm-3)
wasflat, independent
of the heat treat-ment
(the
sulfur out diffusion describedby
B.V.Dutt et al.
[9]
was notapparent),
therefore we havetaken
Ndr
= Cst. = 5 x1015 cm- 3
for the threesamples. Ny
is theequivalent
statedensity
of thevalence band
(for my*
= 0.85 mo,N y (300 K) =
1.93 x
1019 CM- 3, Nv (77 K)
= 2.56 x1018 cm- 3 ) ; g
represents the
degeneracy
factor of a shallow accep- torlevel,
in the valence band structure of InPWith the
preceeding hypothesis, NZni
andNZns obey
the two relations
Table II presents the values of
NZn, p
andNZns
andNz.,
for thecrystals
50 and 148 before and after heat treatment.2022 For the
sample
50 T the relations 2 and 3 cannot be valid becausethey
lead towhich is
impossible.
2022 For the other
samples
thecalculated p = f (T )
variations
(relation (1)) completely desagree
withthe
experimental results, especially
the saturation of carrierdensity
near 300 Kexpected
from the shallowZn level is not observed. This fact indicates also that the model of electrical activation of Zn is not valid.
- In conclusion neither the Zn out diffusion model nor the Zn activation model can account for
our
experimental
observations. It seems that thepresence of other
deeper
acceptors would be neces- sary toexplain
both results before and after heat treatment. Such levels would notparticipate
toradiative recombinations as indicated
by
luminesc-ence measurements so an
arbitrary
choice of theirenergy level and
density
to account forthe p
=f (T)
measurements would be unrealistic.
3.2 CARRIER LIFETIME PROFILE. - This parameter has been deduced from the forward I V character- istics of S diffused
n+ /p
mesadiodes,
in thepolarization
range ofgeneration-recombination
con-duction.
Figure
2 presents the roomtemperature
forward1 V characteristics for diffused
junctions
realized onCNET-50 substrate : diodes
S3
andS32
are shallowjunctions (xj
103BCm) ;
diodesS31
andS36
aredeeper
(xj
> 103BCm).
Theideality
coefficient n is constantn = 2 in the whole bias
voltage
range for shallow diodes whereas it isequal
tounity (diffusion
conduc-tion)
athigh injection
fordeeper
diodesshowing
thebetter
quality
of these last ones.The forward current
density
can then be written :in which
J0 GR
andJo D
arerespectively
the preexpo- nial terms of G-R and diffusion currents. In thevoltage
range in which n =2, generation-recombi-
nation
(G-R)
was confirmedby
a temperaturestudy : figure 3(a)
shows the forward I-V character-istics of the shallow diode
S32
between 300 and353 K.
Figure
3b shows the variation ÔfI0 G-R
vs.103/ T ;
the deduced activation energy value is about 0.7 eV(half
energy gap(Eg ) value).
Therefore the G-R lifetime TG_R can be deduced from these I-V measurements[10]
and arereported
on table III andfigure
4. The TG_R values arestrongly dependent
onjunction depth, they
increase withxj.
Thegood quality
ofdeep junction
is confirmedby
the domin-ant diffusion current observed at
high injection (J >
1mAlcm2).
On our best diodes thisquality
wasassociated to a low dark reverse current :
jo.9 V. _ 10 - 7 AIcm2, VB :
breakdownvoltage equal
Table II. - Substitutional and interstitial Zn densities
Zns, Zni
deducedfrom
SIMS and 300 K Halleffect
measurements in the case
of
a Zn electrical activation model.1163
Fig.
2. - Room temperature forward I-V characteristics for mesa sulfur diffusedn+ /p
InP diodes with variousjunction depths.
Substrate 50
to 14 V in
agreement
with theempirical
relationgiven by
Sze[10].
Similar results have been obtained
by comparing
the diodes
S47 (xj
= 0.803BCm)
andS49 (xj
= 2.1503BCm)
made
by diffusing
S into the substrate 148.Figure
5presents
their room temperature forward character-istics,
theideality
coefficients observed on variousmesa diodes
S47
vary from 1.66 to 2 whereasn = 1 is
only present
on the diodeS49
in thehigh voltage
range. The TG.R values in this substrate 148are very similar to those determined on the substrate 50
(see
Tabl.III)
forequivalent junction depth ; they
decreaseby
one order ofmagnitude
when thejunction depth
increases from 0.8 to 2.15 F£m. The increase ofJoD in
this substrate with respect to theFig.
3. -a)
Forward I-V characteristics at various tem-peratures Diode S32.
b)
IOG.R versus103 / T
for diode 532.substrate 50 can be related to the
higher doping
levelof this last one.
The forward characteristics of these 700 C sulfur diffused
junctions
can becompared
to those of A.Yamamoto
[11]
fabricated at 625 C on a p type substrate(p =1016 cm- 3 ).
On mesa diodesxj =
0.3 03BCm, thèse authors have observed n =
1.29,
J0 = 1.23 10-13 a/cm2.
3.3 DIFFUSION LENGTH PROFILE. - The detailed
photoelectrical study
of substrate 50 has been madeTable III. - Electrical parameters
of
somen+/p sulfur diffuse
InPjunctions.
Fig.
4. - Generation-recombination lifetime bG-R as afunction of
junction depth
in sulfur diffusedn+ /p
InPdiodes
(substrate
50 : e, substrate 148 :1 ).
and allows to deduce the
Ln profile
in this heat treated substrate.- Schottky
diodes. - TheLn profile
has beendeduced from the
analysis
of theefficiency
of semi-transparent
Au/heat treated p InPSchottky
diodesFig.
5. - 300 K forward 1 V characteristics of sulfur diffused n+/p
InP 148 diodes1165
realized at various
depths
into thesubstrate,
ob-tained
by
controlledetching using
0.5 % Br-methanol
(etching
rate - 0.7>m/min).
The evapo- ratedgold
dots were 80 A thick with a diameter of 360 tjbm. In aSchottky diode,
the internal collectionefficiency
TJ can be written :the first term of the sum
represents
the contribution of the neutralsubstrate,
the second the contribution of the spacecharge region ; a
is theabsorption
coefficient. This relation shows that for a
given
avalue, Ln
can be deduced from the variation of 77 versus w(that
is to say versus the reversevoltage).
The modulated
light (À
= 0.85 lim, a =1.85 x
104 cm-1,
P = 5>W)
is deliveredby
a GaAslight emitting
diode(LED).
The modulated(1000 Hz)
inducedphotocurrent
is measuredthrough
a load with a lock-inamplifier. Figure 6
. presents the
experimental
relative valuesn 1 (- V)/ï?i(0)
as a function of w and the calculatedcurves
giving
the best agreement withexperiment.
The
Ln
values as a function ofdepth
arereported
onfigure
7a. On the samefigure
the TG-Rprofile
is alsopresented.
Two remarks can be made :1)
The Tn values deduced fromLn
andJo D
valuesfor
equivalent junction depths (see
Tab.III)
for thesubstrate 50 agree with TG_R values. This result can be related to the fact that S diffusion does not
degrade
the substrate material.2)
The variations ofLn
and T versusXj
aresimilar, indicating
that themobility
ofminority
carrier ishomogeneous
into the heat treated substrate.Fig.
6. -Expérimental
and calculated variations of~i(-v) ~i(0) = f(w)
for the fourSchottky
diodes(À
= 0.8503BCm).
Fig.
7a. - Ln andJ UO-R proûles
in the substrate 50 for adepth
5 >m.Fig. 7b. - Ln values deduced from EBIC measurements
on diode
S».
,EBIC measurements have allowed to deduce the
Ln
valuesdeeper
into the substrate. The determi- nation arereported
infigure
7b. The heat treatment seems todegrade
thephotoelectrical
parameterLn
more than 10 J.1.m far from the surface. The bulk value(Ln
= 12J.1.m)
is normal for untreated p InP ofequivalent doping
level[12].
- S
diffused
n+/p
diodes. - Theefficiency
of anhomojunction
is due to thephotoresponse
of threeregions :
the front diffused n+region,
the spacecharge region
localized in the lessdoped
pregion (the doping
level in the n diffusedlayer
is ashigh
as2 x
1018 cm- 3),
and the base. In thephoton
energy range 1.27-1.35eV,
in which a isweak,
the contri- bution of the base is dominant and il isequivalent
to :
Figure
8presents
the variationof ni i 1 (V
=0 )
as afunction
a -1
for the shallowjunction S32 . a -1 being
deduced from the data
given by Seraphin [13].
TheFig.
8. -11 i 1= f (« -’)
for thehomojunction S32.
. :
expérimental points
°: linear variations for Ln = Cst
---- : calculated variation for the Ln
profile
offigure
7.experimental points
do not follow the linearexpected
variation in the case of a constant
Ln
value(full line).
An agreement betweenexperiment
and calcu-lation has been obtained
by taking
into account theLn profile
infigure 7 ;
a numerical resolution ofcontinuity equation
for electrons was in this casenecessary and the calculated
rl î 1
variation is re-ported
infigure
8(broken line).
Thisspectral
re-sponse allowed to
investigate
the diffusionlength profile
15 f.Lm far from thejunction.
The
study
of the relativevariation q i (- V) / "., i (0)
as a function of w for À = 0.85 >m has allowed to
precise
theLn profile
in a restricted range near the spacecharge edge. Figure
9presents
the exper- imental determinations and the calculated variation(broken line) taking
into account theLn profile
infigure
7. Thegood agreement
betweenexperiment
and calculation confirms the
validity
of the diffusionlength profile : Ln
= 0.3 )JLm near the surface andLn
> 4 >m at adepth
of 3 03BCm.3.4 DEEP LEVEL TRANSIENT SPECTROSCOPY
(DLTS)
MEASUREMENT. - Thetraps
will be de- notedHTI.
Thetype
of measurement have beenperformed
in order to find apossible
correlation between the carrierdensity
and the presence ofdeep
Fig. 9. 2013 7?i(- V) = W
for homojunction 32’
. :
expérimental points
: constant diffusion length Ln model
---- : calculated variation with the Ln profile of
figure
7._
traps. The behaviour of
crystals
50 and 158 and thatof
crystal
148 arestrongly
different.- Substrates 50 and 158. - DLTS measurements
on heat treated substrate 158 reveal two hole traps
HTT1
andHTT2
withrespective energies : E,
+ 250 meV andE,
+ 475 meV andcapture
cross sections : 1.5 x10-17 CM2
and 2 x1O-12 cm2.
On heat treated substrate50, HTT1
isonly
present.These
traps
are not detected into as growncrystals
so we can conclude that
they
have been introducedby
heat treatment. We haveinvestigated
in moredetail the
profile
of theHTT1 trap using
double DLTS(DDLTS)
measurements.Figure
10 shows that thistrap desappears
at adepth
of 0.2 ktm.Analog
behaviour was observed on
HTT2 trap.
Measurementson
deep Schottky
diodesconfirm,
that notrap
ispresent
in the bulk of the heat treated substrates. In S diffuseddiodes,
in which the traps are observeddeeper
into thecrystals (xj
> 0.2p,m ),
no additionaltrap
has been detected. This observation showsthat,
S diffusion does not introduce
trap.
The energy level of
HTT2
is similar to that of thetrap
observedby
C.C.D.Wong [5] : (Et
= 434meV,
1167
Fig. 10. - Deep level
Hrr, profile
into heat treatedcrystal 50.
Ut = 3.2 x
10-14 cm2) :
but its capture cross section is very muchhigher: uHm
= 2 x10-12 cm2.
HTT2
is also different from thedeep
holetrap (522 meV) [14, 15]
observed on Siimplanted
andannealed n+
/p
InP 158junctions.
The DLTS resultson
simply
annealed p InP confirms that the 522 meVtrap
was introducedby implantation.
- Substrate 148. - DLTS measurements have not been
possible
on thehighly
resistantcrystal
148 A.
On the heat treat
crystals
four traps are detected.Figure
11presents
thetypical
DLTS scan, and theparameters of the observed traps.
The difference between the
magnitudes
of theHTT4
traps onsamples
Sch10 and S49 does notcorrespond
to a net difference in trapsdensities,
it is due to the greater holedensity
into the S49sample (see
Tabl.I)
asAC/C
ocNt/2 (Na - Nd ).
The four traps are
present
both at the surface andin the bulk of all the
samples indicating
thatthey
areprobably
native defects. The trapsHTT4
could becompared
to the hole trap(Et
= 480meV,
U 00
=10-13 CM2)
observedby
G. Bremond[16]
in p type InP and thetrap HTT5
to the trap detectedby
SSLi et al.
[17]
into Zndoped
InP Some authors[18]
have
reported
that substitutional Zn could be as-sociated to native
defect,
the lack of DLTS measure-ment on as grown 148 substrate does not allow to attribute the hole increase to a dissociation of such a
complex.
The absence ofdeep
traps in the bulk of as grown and heat treatedcrystals
50 and 158 does not allow to attribute the hole increase to thisphenomenon.
Fig.
11. - DLTS scan of heat treated 148crystals
asobserved on various devices, table of the traps parameters.
4. Conclusion.
Electrical and
photoelectrical parameters (hole
den-sity
p, lifetime T, diffusionlength Ln)
in Zndoped
InP substrates are
strongly
modifiedby
a 700 C heattreatment
during
time of half an hour or several hours. The holedensity
increase(more
than oneorder of
magnitude)
ishomogeneous
into the sub- strate. The Znexodiffusion,
Zn electrical activation and the dissociation of a Zncomplex
failed toaccount for this increase. The variations of T and L
as a function of
depth
into the heat treatedsamples
indicate a strong
degradation
of the material nearthe surface. Such a behâviour
impedes
the realization of efficient shallow diodes for solar energy conver- sioninvolving
heat treatment(T
=700 °C )
on thistype of InP substrate.
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KAWAKAMI, T., OKAMURA, M., Electron. Lett. 15(1979)
502.[2]
KIM, O. K., FORREST, S. R., BONNIER, W. A., SMITH, R. G.,Appl. Phys.
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