IEEE TRANSACTIONS ON ELECTRON DEVICES, VOL. 61, NO.

11, NOVEMBER 2014 3625

Characterization of the Depth Distribution and

Electrical Activation and Deactivation of
Ion Implanted Dopants in Silicon
Shu Qin, Senior Member, IEEE

Abstract— Electrical-assisted diffusion of carriers is pro- However, there are several arguments against this theory.
posed as a hypothesis of major dopant deactivation kinetics. First, because of a very small percentage of the activated
New metrology methods, including SIMS/ARXPS and continuous dopant (carrier) concentration to the Si atomic density, the
anodic oxidation technique/differential Hall effect methods, are
used in this paper to supply supporting evidences and data. probability of cluster or precipitate formation is very small.
The n-type (P- and As-based) implants show more serious For example, the maximum activated B, P, or As dopants
deactivation, but similar reactivation to p-type (B-based) are limited by their electrically active solid solubility, which
implants, which can be interpreted by the electrical-assisted is only ∼2–4 × 1020 /cm3 concentration after a 1000-°C
diffusion mechanism. Reactivation occurs only when the excess anneal [8], [9]. It is much <1% of the Si atomic density, which
dopants exist—dopant concentration is higher than its electrically
active solid solubility limit. is 5×1022 /cm3 [10]. Therefore, the published cluster evidences
shown by HR-TEM images are suspicious. Second, only a
Index Terms— Concentration-dependent diffusion, deacti- limited amount of evidences and data exists on this subject,
vation, electrical-assisted diffusion, electrically active solid
solubility, reactivation, segregation. providing an inconclusive look into the cluster or precipitate
mechanisms. Proposed cluster or precipitate mechanisms were
I. I NTRODUCTION based on the existing metrology measurements available at
that time. Conventional SIMS method was used to determine
T HE requirement for ultrashallow junctions to include
improved R S − x j characteristics, reasonable junction
abruptness, and lower junction leakage to realize source and
impurity dose. Conventional spreading resistance profiling
(SRP), or Hall, or differential Hall effect (DHE) methods were
used to determine activated dopant (carrier) dose. However,
drain (SD) and SD extension (SDE) in Si complementary
the conventional SIMS method may overestimate impurity
metal–oxide–semiconductor (CMOS) devices has resulted in a
doses in Si substrate because it cannot decouple oxide (neither
broad use of low-energy implants and an increased variety of
native oxide nor cap oxide) with Si substrate, in addition to
annealing processes [1]. A very high degree of dopant elec-
its fundamental artifact issues, such as transient and matrix
trical activation is required because the sheet resistance (R S )
effects [11]. Therefore, the diffusion and segregation phe-
of SD and SDE regions has to be maintained at a low level.
nomena in the native oxide were not taken into account.
However, it is well-known that high concentrations of dopant
Conventional SRP or Hall methods may underestimate carrier
are easily deactivated when subjected to subsequent thermal
doses due to their physical issues and limits [12]. Dopant
treatments between 500 °C and 800 °C for a relatively long
(carrier) loss mechanisms might be misled and misunderstood.
time between a couple minutes to hours of the furnace-based
Dopant deactivation is caused by the carrier loss mechanism
processes. When that happens, R S is significantly increased
[2]–[7] during low T and long t thermal treatments. The
and CMOS device performance is significantly degraded.
carrier loss strongly depends on annealing process condi-
The typical low temperature (T ) and long-time (t) thermal
tions, the manner of annealing such as furnace-based, RTP
treatments are the backend processes after SD and SDE have
(rapid thermal process), or laser-based, temperature and time,
been formed, including depositions of variety of the dielectric
and ambient control (O2 residue control). Different dopants
or metal films by CVD, PECVD, or PVD processes. In recent
show very different characteristics [8], [9] on concentration-
decades, several experimental results and first principle calcu-
dependent diffuse-in into Si substrate, diffuse-out via oxide,
lations have suggested that the main mechanism behind this
electrical-assisted diffusion, and segregation (redistribution)
deactivation is the clustering of activated dopants (carriers)
behaviors at SiO2 /Si interface. For example, diffusivities of
or precipitates formed with access vacancy or interstitial
As, P, and B in SiO2 and in Si are very different [14], [15],
concentrations [2]–[7].
and As, P dopants have opposite segregation behaviors to
Manuscript received March 6, 2014; revised June 23, 2014; accepted B [14], [15]. Dopant or carrier dose in Si is a competition
July 22, 2014. Date of publication August 19, 2014; date of current and balance of diffuse-out (loss), electrical-assisted diffusion
version October 20, 2014. The review of this paper was arranged by
Editor H. S. Momose. (loss), segregation (loss or gain), and diffuse-in (gain) under
The author is with Micron Technology Inc., Boise, ID 83707 USA (e-mail: solid solubility limit.
sqin@micron.com). In this paper, a new method, SIMS/ARXPS method [11]
Color versions of one or more of the figures in this paper are available
online at http://ieeexplore.ieee.org. is used to associate with electrically active solid solubility
Digital Object Identifier 10.1109/TED.2014.2342535 to determine impurity and activated dopant doses in both
0018-9383 © 2014 IEEE. Personal use is permitted, but republication/redistribution requires IEEE permission.
See http://www.ieee.org/publications_standards/publications/rights/index.html for more information.

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3626 IEEE TRANSACTIONS ON ELECTRON DEVICES, VOL. 61, NO. 11, NOVEMBER 2014

native oxide and Si substrate. The decoupling of the native

oxide with Si substrate and minimizing the SIMS artifacts
lead to more accurate results. A new method, continuous
anodic oxidation technique (CAOT)/DHE [12], [13], is used
to determine carrier concentration, dose, and mobility in
Si substrate. Its unique features provide more accurate results.
Closer correlations among nonactivated dopant and activated
dopant doses, electrical carrier dose, mobility, and R S data can
be achieved and studied.
II. E XPERIMENT AND D ISCUSSION
Single-crystalline (100)-oriented p-type or n-type Si blan-
ket wafers were processed by phosphorus and boron
implants with high-dose and low-dose conditions, respectively.
High-dose implant is conducted to make its impurity con-
centration higher than its electrically active solid solubility
PSS or BSS . Low-dose implant is conducted to make its
impurity concentration lower than PSS or BSS . After implants,
the wafers were processed with a standard postimplant
strip/clean procedure, and then annealed by a sequence of
1RTP 1000 °C/20 s + 2Anneal 680 °C/104 min + 3RTP
1000 °C/20 s thermal treatments, and all of them are in N2
ambient. The 2Anneal 680 °C/104 min was used to mimic
the total thermal budget (Dt) of the backend processes. Sheet
resistance (R S ) was measured by 4 point-probe (4PP) and Hall
(van der Pauw structure) methods. Impurity profiles and doses
were measured by SIMS/ARXPS methods for each thermal
treatment step. Carrier (electron or hole) concentration, dose,
and mobility were measured by CAOT/DHE method for each
thermal treatment step. Fig. 1. SIMS/ARXPS P profiles of P implants with 15-keV energy, high-
dose (4 × 1015 /cm2 ) (top), and low-dose (5 × 1014 /cm2 ) conditions (bottom)
Fig. 1 (top) plots the impurity profiles and doses of each on as-implanted and annealed Si wafers.
process steps using SIMS method, and illustrates dopant loss
mechanisms. Activated P or carrier doses can be defined and
measured by SIMS profile under PSS (P electrically active solid is higher than PSS , and that of low-dose implant is lower
solubility level) or CAOT/DHE method. Dopant loss occurs by than PSS .
competition and balance of concentration-dependent diffusion High-dose implant shows more diffuse-in during Dts by
(diffuse-out and diffuse-in), electrical-assisted diffusion, and higher concentration-dependent diffusion, due to both higher
segregation at each thermal budget. P concentration gradient and excess P above PSS . Low-dose
implant shows almost no change of profiles due to much
A. Phosphorus Implants less diffuse-in (lower P gradient and no excess P). Both
Table I lists and summarizes the experiment matrix and implants show monotonic decreasing P doses in Si versus
results of the phosphorus implants. Fig. 1 plots and com- subsequent Dts. Listed in Table I, 2Anneal (680 °C/104 m)
pares P SIMS/ARXPS profiles for P implants with 15-keV shows more P in oxide for high-dose implant by electrical-
energy, (top) high-dose (4 × 1015 /cm2 ), and (bottom) assisted diffusion and causes deactivation. However, 2Anneal
low-dose (5 × 1014 /cm2 ) conditions on as-implanted and of low-dose implant does not show this effect.
annealed Si wafers, respectively. SIMS measurement utilized Fig. 2 illustrates a comparison of sheet resistance (R S )
Cs primary beam with an energy of 2 keV at normal inci- versus anneals for both high-dose and low-dose P implants.
dence. The native oxide thickness was separately measured by There are two R S values, which are measured by 4PP and
ARXPS and listed in Table I. P doses in the native oxide and Si Hall (van der Pauw structure) methods, respectively. Fig. 3
substrate for the as-implanted, and each Dt are measured and illustrates a comparison of dopant doses in Si substrate versus
calibrated by the SIMS/ARXPS method and listed in Table I. anneals for both high-dose and low-dose P implants. There
Because ARXPS is not a sputtering-based method, the artifacts are two dopant dose values, P dose and carrier (electron)
caused by the conventional SIMS method, including transient dose, which are measured by SIMS/ARXPS and Hall methods,
and matrix effects, can be minimized. Accurate impurity respectively. Fig. 4 illustrates a comparison of dopant doses
doses in both native oxide and Si substrate can be quantified. in SiO2 (native oxide) versus anneals for both high-dose and
The dose variations of P dopants in both native oxide and low-dose P implants.
Si substrate for each process are also listed for comparison. Several interesting features have been observed in
As shown in Fig. 1, P concentration of high-dose implant Figs. 2–4. First, high-dose implant shows serious deactivation

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QIN: DEPTH DISTRIBUTION AND ELECTRICAL ACTIVATION AND DEACTIVATION OF ION IMPLANTED DOPANTS IN SILICON 3627

TABLE I
P HOSPHORUS I MPLANT E XPERIMENT M ATRIX AND R ESULTS

Fig. 2. Sheet resistances (4PP R S and Hall R S ) versus anneals for both Fig. 4. P dopant dose in SiO2 (native oxide) versus anneals for both
high-dose and low-dose P implants. high-dose and low-dose P implants.

decreases of 8.9%, attributed to electron dose increase 1.5%

Fig. 3. P dopant dose and electron dose in Si substrate versus anneals for
both high-dose and low-dose P implants.
at 2Anneal 680 °C/104 m—R S increases 22%, attributed to
electron dose decrease 38.3%. Then, reactivation occurs at
3RTP 1000 °C/20 s—R S decreases 25.3%, attributed to elec-
tron dose increase 64.5% referring to 2Anneal, and a net R S
and mobility increase 9% referring to 1RTP. However, low-
dose implant does not show significant deactivation and reac-
tivation due to much less diffusion, occurring from the lower
P concentration gradient and P concentration lower than PSS .
Second, in contrast to electron dose, P impurity dose in Si
monotonically decreases versus Dts for both implants. Third,
a very good consistence between 4PP R S and Hall R S , and a
correct correlation between R S and electron dose have been
demonstrated. This also confirms that the Hall measurement
data, including electron dose and concentration and mobility
results are very reliable.
Table I lists junction depth x j versus anneals for both
high-dose and low-dose implants. High-dose implant shows
more diffuse-in during Dts by higher concentration-dependent
diffusion due to higher P concentration gradient. Low-dose
implant shows almost no change of profiles due to much less
diffusion (lower P gradient). Fig. 5 illustrates a comparison
of carrier mobility µ versus anneals for both high-dose and
low-dose P implants. Mobility is a function of impurity or
carrier concentration, so that high-dose implant shows lower
µ than low-dose implant. High-dose implant at 2Anneal shows

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3628
Fig. 5. Carrier mobility µ versus anneals for both high-dose and low-dose
P implants.
higher µ than that at 1RTP due to lower carrier concentration
caused by deactivation. Low-dose implant shows similar but
not significant due to less deactivation.
Carrier (electron) loss of high-dose implant at 2Anneal
has at least two components: 1) concentration-dependent
diffuse-out and 2) electrical-assisted diffuse-out. As shown
in Table I, electron dose was lost 7.5 × 1014 /cm2 dose,
∼38.3% at 2Anneal measured by Hall method. P impurity
loss at 2Anneal has at least two components: 1) concentration-
dependent diffuse-out and 2) segregation. P impurity dose in
Si was lost 2.2 × 1014 /cm2 dose, ∼7.1%, during 2Anneal
measured by SIMS method. Because the SIMS P dose in Si
was a mixture of activated P (electron) and nonactivated P,
and the segregation of P impurity at native Ox/Si interface
will gain more P in Si [14], [15], we cannot extract the
activated P (electron) loss from the SIMS P data in Si.
However, the electrical-assisted diffusion of electron can be
quantified by SIMS/ARXPS P dose in the native oxide
because of the positive charges in the native oxide (Dit
and fixed charges). Native oxide is believed to be a dirty
oxide because it is formed in the atmospheric environment.
This mechanism is confirmed by SIMS/ARXPS P(Ox) dose
increase 6.12 × 1014 /cm2 , ∼54.5% at 2Anneal, as shown in
Table I and Fig. 4. Although we cannot quantify electron loss
from its diffuse-out component, 6.12 × 1014/cm2 electron loss
measured by SIMS/ARXPS method is fairly consistent with
7.5 × 1014 /cm2 electron loss measured by Hall method if the
electron loss from diffuse-out component is included. Besides,
such low T at 2Anneal cannot diffuse-in and activate more
P from the excess P. Therefore, a net effect is electron loss
and deactivation. Electrical-assisted diffusion mechanism is a
mutual and/or combination of the electrical Coulomb force
and the concentration-dependent diffusion. The electron loss
mechanism of electrical-assisted diffusion also can explain
why p-type doping shows less deactivation phenomenon than
n-type doping because hole has positive charge and shows
an opposite effect to electron on electrical-assisted diffusion.
This phenomenon will be demonstrated in Section II-B, and
had been shown in [16] and [17]. Significant reactivation
occurs at 3RTP 1000 °C/20 s. R S decreases 25.3% referring
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IEEE TRANSACTIONS ON ELECTRON DEVICES, VOL. 61, NO. 11, NOVEMBER 2014
to 2Anneal, and a net R S decreases 11.1%, referring to 1RTP.
During 3RTP, electron increases 7.8×1014/cm2 dose, ∼64.5%
referring to 2Anneal, and a net 3 × 1013 /cm2 electron dose
increase ∼1.5% with mobility increase ∼9% referring to 1RTP
by more P diffuse-in and more activation from the excess P at
higher T after a compensation of the electron loss at 2Anneal.
Low-dose implant does not show significant deactivation and
reactivation due to much less diffusion occurred from the lower
P gradient and P concentration lower than PSS .
B. Boron Implants
Table II lists and summarizes the experiment matrix and
results of the boron implants. Fig. 6 plots and compares B
SIMS/ARXPS profiles for B implants with 7-keV energy,
high-dose (5 × 1015 /cm2 ), and low-dose (5 × 1014 /cm2 ) con-
ditions on as-implanted and annealed Si wafers, respectively.
SIMS measurement utilized O2 primary beam with energy of
2-keV at normal incidence. The native oxide thickness was
separately measured by ARXPS and listed in Table II.
The B doses in native oxide and Si substrate for the
as-implanted and each Dt are measured and calibrated by
SIMS and listed in Table II. The dose variations of B dopants
in both native oxide and Si substrate for each process are also
listed for comparison. High-dose implant shows more diffuse-
in during Dts by higher concentration-dependent diffusion due
to both higher B concentration gradient and excess B dopant
above BSS . Low-dose implant shows almost no change of
profiles due to much less diffuse-in (lower B concentration
gradient and no excess B).
Listed in Table II, 2Anneal (680 °C/104 m) shows slightly
more B in both oxide and Si substrate for both implants, which
are very different to n-type (P- and As-based) implants. The
mechanism will be discussed in detail later.
Fig. 7 illustrates a comparison of sheet resistance (R S )
versus anneals for both high-dose and low-dose B implants.
There are two R S values, which are measured by 4PP and
Hall (van der Pauw structure) methods, respectively. Fig. 8
illustrates a comparison of dopant doses in Si substrate versus
anneals for both high-dose and low-dose B implants. There are
two dopant dose values, B dose and carrier (hole) dose, which
are measured by SIMS/ARXPS and CAOT/DHE methods,
respectively. Fig. 9 illustrates a comparison of dopant doses
in SiO2 (native oxide) versus anneals for both high-dose and
low-dose B implants.
Differing from n-type (P- and As-based) implants, sev-
eral interesting features have been observed in Figs. 7–9.
First, high-dose implant shows little deactivation at 2Anneal
680 °C/104 m—R S only slightly increases 5.43%, attributed
to hole-dose slight decrease 2.54%. Then, reactivation occurs
at 3RTP 1000 °C/20 s—R S decreases 16.7%, attributed to
hole-dose increase 12.9% referring to 2Anneal, and a net
R S decreases 12.2%, attributed to hole dose increase 10%
referring to 1RTP. Second, in contrast with hole doses,
B impurity doses in Si slightly increase at 2Anneal then
decrease at 3RTP. Third, a very good consistence between
4PP R S and Hall R S , and a correct correlation between R S
and hole dose have been demonstrated. This confirms that the
QIN: DEPTH DISTRIBUTION AND ELECTRICAL ACTIVATION AND DEACTIVATION OF ION IMPLANTED DOPANTS IN SILICON 3629

TABLE II
B ORON I MPLANT E XPERIMENT M ATRIX AND R ESULTS

Fig. 7. Sheet resistances (4PP RS and Hall RS ) versus anneals for both
high-dose and low-dose B implants.

Fig. 6. SIMS/ARXPS B profiles of B implants with 7-keV energy, high-dose

(5 × 1015 /cm2 ) (top), and low-dose (5 × 1014 /cm2 ) (bottom) conditions on
as-implanted and annealed Si wafers.

Hall measurement data, including hole dose and concentration
and mobility results are very reliable.
Table II lists junction depth x j versus anneals for both
high-dose and low-dose implants. High-dose implant shows
more diffuse-in during Dts by higher concentration-dependent
diffusion due to both higher B concentration gradient and
excess B above BSS . Low-dose implant shows almost
Fig. 8. P dopant dose and electron dose in Si substrate versus anneals for
both high-dose and low-dose B implants.
no change of profiles due to much less diffusion (lower B
concentration gradient and no excess B).
Fig. 10 illustrates a comparison of carrier mobility µ
versus anneals for both high-dose and low-dose B implants.
Mobility is a function of impurity or carrier concentration,

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3630 IEEE TRANSACTIONS ON ELECTRON DEVICES, VOL. 61, NO. 11, NOVEMBER 2014

charged activated B (hole) into Si. Therefore, a net B increase

in Si at 2Anneal is a balance of the B loss from diffusion-out
and segregation and B gain from electrical-assisted diffuse-in.
The electrical-assisted diffusion of hole also can be quanti-
fied and confirmed by SIMS/ARXPS B dose in the native
oxide. SIMS/ARXPS measured B dose in oxide only increase
9.1 × 1012 /cm2 , ∼9% at 2Anneal, as shown in Table II
and Fig. 9. Comparing with 54.5% P(Ox) dopant increase
in oxide of the n-type doping cases, 9% of B increase in
oxide is also a net balance of diffusion-out, segregation, and
electrical-assisted diffusion. The phenomenon of the p-type
doping showing less deactivation than n-type doping had been
published elsewhere [16], [17].
Based on the activation and deactivation data of
P- and B- implants, we can define and calculate an activation
Fig. 9. B dopant dose in SiO2 (native oxide) versus anneals for both fraction as the total carrier dose divided by the SIMS activated
high-dose and low-dose B implants.
impurity dose. The activated impurity dose is defined and
calculated by integrating the SIMS impurity profile beneath
solid solubility. The activation fractions of P-implanted and
B-implanted Si are listed in Tables I and II, respectively. The
P-implanted Si shows an activation fraction ≤70%, and ∼40%
at 2Anneal due to deactivation. The B-implanted Si shows an
activation fraction of >100%, even at 2Anneal due to less
deactivation. These data are very consistent to those published
in [13]. An activation fraction of >100% is abnormal. It was
caused by the artifact or error of the solid solubility data,
which was measured by the conventional SIMS method and
based on the diffusion doping method. A comparison of
the activation fractions of the P-implanted and B-implanted
Si demonstrates evidence of the electrical-assisted diffusion
mechanism.

III. C ONCLUSION
Fig. 10. Carrier mobility µ versus anneals for both high-dose and low-dose
B implants. Characterization of the depth distribution and electrical
activation and deactivation of ion-implanted dopants in silicon
demonstrates that electrical-assisted diffusion of carriers could
so that high-dose implant shows lower µ than that of low-
be a hypothesis of a major dopant deactivation kinetics. New
dose implant. Differing from n-type doping, both high- and
metrology methods, including SIMS/ARXPS and CAOT/DHE
low-dose implants at 2Anneal do not show higher µ than that
methods, are used in this paper to supply supporting evidences
at 1RTP due to little deactivation occurred.
and data. N-type P implants show more serious deactiva-
Carrier (hole) loss of high-dose implant at 2Anneal
tion, but similar reactivation to p-type B implants, which
680 °C/104 m has at least two components: 1) concentration-
can be interpreted by the electrical-assisted diffusion mech-
dependent diffuse-out and 2) electrical-assisted diffuse-out.
anism. Reactivation occurs only when the excess dopants
As shown in Table II, hole dose was lost 5.4 × 1013 /cm2
exist—dopant concentration is higher than its electrically
dose, only ∼2.54% at 2Anneal 680 °C/104 m measured
active solid solubility limit.
by Hall method. B impurity loss at 2Anneal has at least
two components: 1) concentration-dependent diffuse-out and
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Shu Qin (M’94–SM’97) received the Ph.D. degree
in electrical engineering from Northeastern Univer-
sity, Boston, MA, USA.
He has been a Senior Member Technical Staff
with Micron Technology, Inc., Boise, ID, USA,
since 2004. His current research interests include
advanced semiconductor processing, novel plasma
sources and plasma diagnoses, and device and
process simulations. He holds more than 40 U.S.
and international patents.