Applications of Surface Science 20 (1984) 167-180 167

North-Holland. Amsterdam

QUANTITATIVE AUGER ELECTRON SPECTROSCOPY AND

RUTHERFORD BACKSCATTERING OF POTASSIUM-IMPLANTED
SILICON, SILICA AND SODIUM TRISILICATE *

Brad J. BURROW ** and Neal R. ARMSTRONG

Department of Chemistry, Unruersity of Arizona, Tucson, Arizona 85721, USA

and

Rod K. QUINN, Bruce C. BUNKER, George W. ARNOLD

and Doug R. SALMI
Sandia Natronal Laboratories ***, Albuquerque. New Mexico 87185, USA

Received 25 May 1984; accepted for publication 2 August 1984

Samples of silicon, silica, and sodium trisilicate, which were ion implanted with potassium,
were analyzed by Auger Electron Spectroscopy (AES) and Rutherford Backscattering Spectros-
copy (RBS). Depth profiles obtained by both techniques showed that approximately 50% of the
implanted potassium migrated from the subsurface implant region to the surface for both the silica
and sodium trisilicate samples. Less migration was detected for the silicon samples. Analyses of the
results suggest that some of the ion migration observed in Auger depth profiles is induced by the
analysis technique. With this exception, it is demonstrated that a combination of AES and RBS
techniques can provide quantitative compositional analyses for altered glass surfaces.

1. Introduction

Reactions of silicon, silica and silicate materials with active metals such as
lithium, sodium or potassium are of interest in the chemistries of a variety of
energy storage battery systems using alkali metal anodes [l-S]. Alkali metal
anodes act as high energy density reducing agents in the battery discharge
reaction. Their reducing strengths can pose a severe problem in their contain-
ment. Materials such as atmospheric gases, electrolyte, current collectors, and
battery containers that interface with the active metal are subject to corrosion

* This work partially performed at Sandia National Laboratories supported by the US Depart-
ment of Energy under Contract No. DE-AC04-76DPOO789.
** Present address: US Phillips Research Laboratories, Sunnyvale. California, USA.
*** A US DOE facility.

0378-5963/84/$03.00 0 Elsevier Science Publishers B.V.

(North-Holland Physics Publishing Division)
and the mechanical failures that result from chemical breakdown [6]. Specifi-
cally, the silicate glass used in hermetic glass-to-metal seals in battery headers
can be eventually destroyed by lithium metal attack. During storage. lithium is
electrochemically deposited on glass surfaces by the reduction of Li’ present
in battery electrolytes by an underpotential deposition mechanism [7.8]. This
lithium metal reacts with silicate-based glasses to form conductive products.
The process continues until the seal is destroyed.
Surface analytical techniques are being used to monitor the course of
corrosion reactions on glasses used in batteries. Simple glass systems are being
characterized first so that the surface chemistries of corroded glass materials
can be understood. Evaporation of thin films of the active metal, which results
in a controlled reaction at the glass surface, is one method of analyzing these
reactions. Ion implantation of a fixed dose of active metal in a near surface
region has also been attempted. This paper describes some of our preliminary
studies and problems encountered in using Rutherford Backscattering Spec-
trometry (RBS) and Auger Electron Spectroscopy (AES) to characterize K+
implanted materials.
The combination of AES and RBS can be a powerful analytical technique.
AES is appropriate for elemental identification of surface species. With careful
background subtraction and deconvolution techniques, chemical bonding in-
formation can be obtained [9]. Quantitative surface analysis by AES is more
difficult because of the dearth of surface standards for calibration [lo-131. We
have investigated the quantitative aspects of AES and applied these techniques
to the analysis of titanium [14-161. The combination of AES and Quartz
Crystal Microgravimetry can quantitatively monitor the formation of titanium
surface oxides [16]. We report here the results of the combination of AES and
RBS in a similar capacity. RBS is both quantitative and depth selective in a
“non-destructive” manner although it is not chemically specific nor particu-
larly surface sensitive. Hence, the two techniques complement each other. By
using noble ion sputtering, the Auger spectrum can also reflect the same depth
profile, provided there is no preferential sputtering or knock-on effects and
that the ion beam or the electron beam does not induce any chemical changes
or diffusion processes.
We describe here our initial application of these techniques to the study of
potassium-implanted silicon, silica glass and sodium trisilicate glass, which are
models for active metal corrosion systems and active metal/silicon alloys.
Electron beam induced reduction of SiO, has been well-documented [17,18]
but can be avoided if the electron beam current density is kept below a
threshold level. Preferential sputtering does not occur in SiO, [19]. In the case
of sodium trisilicate, it has been noted that high energy Arf ions induces Na
migration away from the surface into the bulk [20]. In SiO, and Na,O . 3SiO,,
our results show that the implanted potassium is mobile. The implanted
potassium is difficult to quantitative by AES, probably because of electron-
 B.J. Burrow et al. / K -tmplanted Si, SO, and Nu,O. 3St02 169

beam induced diffusion [21-271. We also describe and expand the application
of AES quantitation techniques reported earlier [16] with certain modifications
necessary to quantitate Auger amplitudes with kinetic energies below 200 eV.

2. Experimental

The three materials chosen for this study were plished, single crystal silicon,
silica glass, SiO,, and sodium trisilicate glass, Na,O . 3Si0,. Potassium was
chosen as the alkali metal for implantation because of its large Auger yield.
Also the large mass of potassium resulted in the desired near-surface ion
implant. The RBS signal for potassium is well resolved from the scattering
profiles of the other components (Si, 0, and Na), and RBS is more sensitive to
K than to the lower 2 components.
Potassium was implanted into the three samples by an Accelerators, Inc.
300 kV accelerator using a plasma source and K&O, as the potassium source.
The implantation energy was 45 keV to give a profile which, in the absence of
diffusional effects, should peak at ca. 500-700 A below the surface. The ion
current fluctuated between 0.5-3.0 PA because of instability of the plasma,
with an average of 1.5 PA. The integrated ion current density was recorded
and converted to the following total ion fluxes: Si (3.5 X lOI K+/cm2), SiO,
(4.0 X 1016 K+/cm2) and Na,O . 3Si0, (3.0 X 10lhK ‘/cm2).
The Rutherford backscattering experiment was conducted using a tandem
Van de Graaff accelerator at Sandia National Laboratories. A 2.8 MeV 4He
ion beam impinged at an angle of 55” to the surface normal; the incident
current was ca. 5 nA. The solid state detector was located at 10” off the surface
plane; the backscattering angle was 155”. These experimental conditions
provided a depth resolution of ca. 150 A.
AES was conducted in a Physical Electronics Thin Film Analyzer with an
incident electron beam of 2.0 keV and a current of 200 nA (nominal beam
diameter was less than 0.1 mm). The analysis time was five minutes per scan.
The electrons were energy analyzed with a single-pass cylindrical mirror
analyzer and collected by an electron multiplier operated in the DC mode.
Direct N(E) . E spectra obtained via an isolation amplifier were digitized and
stored in a DEC LSI-11/23 computer system for later data manipulation, as
described previously [14].
Background subtraction from the Auger data was accomplished using a
two-step process [16]. Fig. 1 illustrates this process in three stages for the
O(KLL) transition. The original N(E). E data (fig. 1A) is composed of (1) an
Auger current spectrum, (2) a background function at kinetic energies higher
than the O(KLL) threshold from electron sources such as the primary beam
and any higher kinetic energy Auger processes, and (3) a lower energy
background which consists of inelastically scattered electrons, other minor
Auger transitions and some electrons from quantized loss processes (e.g., from
surface and bulk plasmons). A background function calculated by a least
squares analysis of the high energy background is extrapolated to lower
energies and subtracted, according to the method of Sickafus [28]. In the cases
reported here, the energy dependence of the analyzer transmission was not
corrected prior to background subtraction. In the past we have always cor-
rected the N(E). E spectrum for the CMA transmission function first, result-
ing in an N(E) spectrum which is independent of kinetic energy [29]. We have
determined that it is not necessary to first correct the data for the transmission
response. Indeed in the case of the low energy silicon spectra, it is advisable to
leave the data in the N(E) . E form to avoid magnification of the spectral noise
at low kinetic energies. This high energy background subtraction leaves the
spectrum shown in fig. 1B.
To remove the low energy background and the characteristic losses. a
spectrum of elastically scattered electrons was recorded at the Auger energy.
This spectrum, with the elastic peak suhtacted [HI, approximates the low-en-
ergy background function for an electron source at the Auger energy. Since the
elastically scattered electrons are from an external source rather than an
internal Auger process, some iterative scaling of the background is done to
bring the low energy region to base-line. The inelastic background and
quantized losses are subtracted at each spectral point to obtain the final
spectrum (fig. lC), which is then corrected for the energy dependence of the
analyzer and multiplier prior to area integration.

425 475 525

KINETIC ENERGY eV

Fig. 1. AES N( E).E spectra of 0 (KLL) from silicon surface during the three stages of
background correction. (A) original spectrum. (B) after log-log linear subtraction of high energy
background. (C) After deconvolution of instrument response function.
 B.J. Burrow et al. / K -rmplanted Si, SiO, and Na,O. 3S10, 171

Ion sputtering/depth profiling of the samples was done with an ion gun
mounted in the AES chamber. The Art ions were accelerated to 2 kV with an
emission current of 25 mA in a background Ar pressure pressure of 3 X 10Ps
Torr. The incident ion current was ca. l-10 PA. Sputtering rates for all three
samples were calibrated using the K implant maximum indicated in the RBS
data, subject to the conditions outlined in the next section.

3. Results

3.1. Rutherford backscattering spectra

The RBS spectra for K-implanted Si, SiO, and Na,O . 3Si0, are shown in
figs. 2A-2B. The potassium implant in silicon revealed a nearly Gaussian
lineshape (fig. 2A) as expected for a high mass ion impinging on low mass
target atoms [30,31]. The RBS spectrum (fig. 2A) showed a diffuse surface edge
as compared to unimplanted Si, reflecting dilution of the Si at the surface by
the K implant. Oxygen was also observed to be present in the RBS spectrum
for K-implanted Si where none was seen for unimplanted Si (not shown). The
silicon surface edge of silica (fig. 2B) also showed a dip in concentration
indicative of a 1 : 1 replacement of Si by K. In contrast, the major change upon
K implantation in the sodium trisilicate RBS spectrum (fig. 2C) was seen in the
Na surface edge, where a nearly complete depletion of Na took place at a

SILICON

ION ENERGY ION ENERGY ION ENERGY

Fig. 2. RBS spectra of potassium implanted into: (A) silicon, K peak area = 3.7X lo-l6 K/cm’;
(B) silica, K peak area = 2.6~ lo- I6 K/c&; (C) sodium trisilicate, K peak area = 3.0 x 10
16K cm2. The horizontal scales represent depth X lo3 A and the vertical scales represent atomic
con&tration X lo** atoms/cm’. The potassium region is expanded in the inset where the
expanded horizontal scale now represents depth X 10’ A and the vertical scale represents atomic
concentration X 102’ K/cm’.
depth near the K-implant maximum. The Na concentration did not attain the
bulk value until beyond the implanted region (ca. 1200 A). Depletion of Na
atoms from the near-surface region was also observed in the RBS spectrum of
unimplanted sodium trisilicate (not shown).
The K depth profiles for silica and sodium trisilicate glass also exhibited the
expected implant maxima at a depth of ca. 700 A. However, the profiles also
exhibited a substantial surface peak, suggesting that a significant fraction of
the original implants migrated toward the surface. Assuming a Gaussian
lineshape for the original implant. the percentage of surface-diffused K in silica
was estimated to be ca. 30-40s of the total, while for sodium trisilicate. the
amount diffusing was estimated at ca. 50-60X. It should also be noted that, in
the case of K-implanted silica, the integrated K-implant peak area (2.6 x 10lh
K/cm2) was substantially lower than the integrated implant ion density
impinging on the target (4 x 10lh K/cm*) (see section 4). In the other two
cases, both parameters agreed with each other within experimental error.

3.2. Auger electron spectra

The Auger spectra of K-implanted Si, SiOz and Na,O . 3Si0, are shown in
figs. 3, 4 and 5, respectively. Fig. 3 shows the Si(LVV), the K(LMM) and
C(KVV), and O(KLL) regions of the spectra for three different points of the
ion beam depth profile of Si. The surface region of K-implanted silica is shown
in fig. 4 and a typical bulk spectrum from sodium trisilicate is in fig. 5.
The K(LMM) spectra overlapped the C(KVV) transitions. Sputtering re-
duced the amount of adventitious carbon for each surface but did not remove

Fig. 3. Auger spectra of K-implanted Si at (A) Si surface. (B) the maximum of the K implant and
(C) bulk Si. From left to right. the transitions are Si(LVV). K(LMM) as well as C(KVV) and
O(KLL). The O(KLL) transition for the surface is l/4 scale for the other O(KLL) transitions.
 B.J. Burrow et al. / K -implanred Si, SiO, and NazO. 3S10, 113

it entirely. The origin of the carbon impurity is uncertain but it may be a result
of carbon emission from the AES sputter ion gun. The additional carbon does
not affect the results in comparison to the unimplanted samples. To obtain a
peak area measurement of potassium, it was necessary to subtract the C(KVV)
lineshape from each spectrum. The lineshape that was used for subtraction was
a simple one-peak asymmetric Gaussian distribution calculated to fit the
C(KW) transition in the reference materials (e.g., pure silicon without the K
implant). No attempt was made to attribute any of the fitting parameters to
specific AES transitions of the C(KW) spectrum. The synthesized reference
C(KW) spectrum was then scaled and energy shifted to align with the
C(KW) peak maximum in the ion-implanted AES spectra. The K(LMM)
spectrum before and after the subtraction is illustrated in all of the K(LMM)
spectra in figs. 3, 4 and 5. The treated spectra were over-compensated for C at
the low end of the K(LMM) energy region because the implantation probably
altered the low energy features of the carbon lineshape relative to C in pure Si.
The baseline, however, was adjusted to reflect that change, and a peak area

20 55 90 M 200 250 300”460 500 540

KINETIC ENERGY
Fig. 4. AES of surface of K-implanted SiO,. Each spectral region has been normalized to each
maximum and does not reflect relative intensities.

I, .

!O 55 90 ” 200 250 300 ” 460 500 540

KINETIC ENERGY
Fig. 5. AES spectrum of K-implanted Na,O.3SiO, near the expected implant region.
174 B.J. Burrow et al. / K-implanted SI, SO, and Na_,O’ 3S10,

measurement was made from the remaining potassium peak.

Three major observations were made from the AES results: (1) Near the
implant region in elemental Si, a noticeable change in the Si(L,.,W) lineshapes
was accompanied by an increase in both the O(KLL) signal and K(LMM)
signals. This is illustrated in fig. 3 in Auger spectra taken at increasing depth
from the surface (A) through the K implant (B) to the bulk silicon (C). (2) A
large amount of potassium accumulated on the silica surface (fig. 4). This
potassium AES signal was the largest for potassium on any of the samples. (3)
There was a large depletion of potassium and sodium ions from the sodium
trisilicate glass as seen from the Auger spectra for both surface and bulk (fig.
5). Potassium was barely detected in all instates while sodium was not detected
at all.

3.3. Quantitation of surface concentrations

It can be assumed that the silicon-to-oxygen ratio observed in the RBS

spectra of the silica is very near that expected for SiO,, whether potassium had
been implanted or not. The RBS spectra of silica can be used to check the
validty of our quantitation procedures for AES. The relative atomic ratios of
silicon and oxygen were calculated from Auger data according to the following
expression:

N,,_‘si ao ‘o l+Ro Eo Mo
_-
(1)
No - r, usi X,, 1 + R si Esi MS, ’

where i is the peak area of the Auger transition, u is the ionization cross section
for that Auger transition, X is the mean electron escape depth for an electron at
that kinetic energy, 1 + R is equal to the backscattering factor, E is the energy
transmission correction for the CMA and M is the electron multiplier gain at
the Auger kinetic energy. Values for these parameters are given in table 1. As

Table 1
Calculated sensitivity factors

AES transition o h 1+i7 E M RSF *I

X lo-l9 cm2) (A)
Si(LW) 31 h’ 3.0 1.48 71 1284 7 d’
18 c,
K( LMM) 8.6 6.0 1.37 240 2021 34
0( KLL) 1.0 10.1 1.28 505 2099 14

a) Relative Sensitivity Factor, for use in calculating atomic ratios only

h, Calculated according to Gryzinski [32].
‘) Calculated according to Vrakking and Meyer [35].
d, Calculated using the corrected value for I+,
 B.J. Burrow et (II. / K - tmplanted Si, SiO, and NoJO. 3SiOz 175

in previous AES studies of metal oxides [16], the AES Si/O ratio was
computed from the calculations of cross sections, escape depths and back-
scattering factors in the literature [32-343. In contrast to earlier results [16], we
found that the calculation for the ionization cross section for the Si L,,, level
by Gryzinski’s method [32] led to an atomic ratio of Ns,/N, = 0.25, exactly
half that expected. A recalculation of the ionization cross section by exprapo-
lating the experimentally measured value of silicon from Vrakking and Meyer
[35] to 2 keV by the power law of E-‘.56 (where E is the primary energy)
provided a ratio of N,,/N, = 0.48, which agrees well with the RBS results and
the expected stoichiometry. This result and previous experiments lead us to
speculate that Gryzinski’s method for calculating L,., ionization cross sections
is in error only at low kinetic energies, since this discrepancy was not noted for
the Ti(LMM) transitions [16].
For purposes of computing the AES/depth profiles, sensitivity factors for
Si and 0 were computed using the SiO, AES spectra discussed above and
assuming that both the RBS and the AES data reflect the true Si/O ratio
without undue damage to the sample. The sensitivity factors for these elements
are listed in table 1. In the case of potassium, surface diffusion and electric-field
enhanced diffusion processes (see below) precluded the direct comparison of
the AES and RBS spectra for the glasses only. The sensitivity factor used for
potassium (table 1) was computed using the formalisms described above. Since
the Auger transition for potassium is in a higher kinetic energy region than
that for silicon, it is expected to be less sensitive to some of the problems
referred to earlier. The resultant AES/depth profiles for Si, SiO, and Na,O .
3Si0, are calculated using these sensitivity factors (figs. 6, 7 and 8). The depth

960 ii
Si
15

‘12

KiSI
9
(x000
6

SPUTTER TIME

Fig. 6. AES depth profile of K-implanted Si. Si/O and K/Si atomic ratios calculated according to
text. Depth scale above profile calibrated by equating the maximum K/Si ratio in the AES depth
profile to the maximum K concentration in RBS. The first point of K/Si is not on scale
(K/Si = 0.031).
176 B.J. Burrmv et al. / K-implanted Si, SiO, and Na,O. 3Si0,

scale for these profiles was calculated by correlating the maximum K con-
centrations in the AES profiles with the maximum K concentration in the RBS
data, whose depth was known with some confidence. This method was re-
peated for the small potassium peak in the depth profile of sodium trisilicate.
and this sputter rate was used for both glass samples. The error in sputtering
rates for the glasses is estimated to be larger than that for the sputtering rate of
silicon.
Several general features can be seen in these depth profiles. For the silicon
sample it can be seen that the surface is oxygen rich as expected for a native
oxide. The oxygen level drops in the subsurface region and then rises again
along with the increase in potassium level (consistent with line-shapes above).

12$x3 400 800 1200 A a,2

I
t SiO2
1.0. ; a10
I
I
o.a- \ . l Cl08

0.06 K&i

a04
I
cl2- : o o KlSi QO2
‘. 0
0 _--------___________ 0
0
0
0 20 60 nlin’
SPUTT:: TIME
Fig, 7, AES depth profile of K-implanted SiO,. The surface pomt of K/Si ia not on scale
(K/Si = 0.8).

0.4 I
1 Silo
0.3 -:, KlSi
\
a2 . '1,
! D
1
0.1 '\ P--.
9 K/St
O '\ /' '\
\.. . _
O ‘20’ 60 min
sP”T& TIME

Fig. 8. AES depth profile of K-implanted Na,O. 3Si0,

 B.J. Burrow et at. / K-implanted Si, SO2 and Na,O’ 3.50, 177

Auger spectra of the K implant region (fig. 3) suggest that much of the
subsurface oxygen is present as SiO,, and that most of the potassium has been
oxidized to form K,O. A comparison of K/Si ratios obtained by RBS and
those obtained by AES do not coincide. The AES spectra show high surface
accumulations of K which do not appear in the RBS spectra, and the K
concentrations in the implant region are an order of magnitude lower in the
AES spectra than in either the RBS spectra or the calculated profile based on
the ion implantation parameters. The AES K profile reflects the extensive
migration and sputtering of K which is associated with Auger depth profiling,
illustrating the problems of obtaining quantitative Auger data for mobile
cations in isolating materials.
The AES and RBS depth profiles for SiO, are quite different from one
another in that the potassium profile in the AES data seems to be concentrated
entirely in the near surface region. No evidence for the subsurface maximum in
concentration was observed. Consistent with the RBS data, the presence of
high concentrations of potassium in the near surface region coincides with the
loss of silicon, leading us to speculate that the potassium is present principally
as K,O in this region. It should also be noted that the potassium concentration
is considerably less than that observed in the Si samples and expected from the
RBS data. In the case of the trisilicate samples, the AES depth profiles do
reveal potassium in the bulk as expected from the RBS data. However, once
again the K levels are considerably diminished with respect to what was
expected from the RBS data.

4. Discussion

The results reported here are the first studies of alkali ion migration in
glasses by the combination of AES and RBS. The most significant conclusion
of these studies is the importance of diffusion of the implanted potassium to
the surface. The AES depth profiles indicate that potassium had migrated to
the surface in all three samples. Silicon shows the least migration; therefore the
original implant maximum is still discernible. In the case of the two glasses, an
implant maximum is barely detected in the sodium trisilicate, and no maxi-
mum is seen in the silica glass. The RBS results also indicated a surface
migration of potassium in both glasses but not in the case of silicon.
Alkali ion migration under the influence of an electron or ion beam has
been noted by many authors [21-27, 36-401. Ohuchi and Holloway have
developed a general model for sodium migration in glasses [41]. Most of these
authors attribute this phenomenon to the Lineweaver mechanism [42]. This
mechanism proposes that an incident electron beam on the surface creates an
electric field because of the deposition of accumulate negative charges at the
penetration depth of the incident electron beam. This electric field induces
178 B.J. Burrow et al. / K-rmpluntrd SI. SIO, and Na,O~.WO,

positive alkali ion migration away from the surface into the bulk after a
dissociation event has occurred. The absence of a Na(KLL) transition in the
Auger spectrum of sodium trisilicate is attributed to this mechanism. Potas-
sium ions with the implant maximum would be expected to behave similarly.
With the glass substrate exposed to liquid nitrogen temperatures and
minimal beam current density, Pantano et al. [21,23] have successfully applied
AES with ion milling to obtain the expected depth profiles of alkali silicate
glasses. These results show a small accumulation of alkali metal in the first 100
A of the surface. This is followed by a region of depleted alkali atoms before
reaching the bulk concentration. The accumulation of alkali ions at the surface
is explained by a weathering reaction of the glass during exposure to the
atmosphere. The alkali ion migration to the surface is similar in this respect to
the migration of Li to the Si surface in Li/Si alloys [l] and helps explain the
migration of potassium to the surface of these samples. Backscattering spectra
of the sodium trisilicate glass have confirmed Pantano et al.‘s description of
alkali depletion from the subsurface region [21,23]. It is this result that leads us
to believe that RBS is capable of monitoring ion migration in glasses under a
variety of conditions.
The silicon and silicate glasses exhibited significant differences in their
behavior to the K implant. Based on the shapes of the K and Na profiles of
Na,O . 3SiO,, the RBS data suggest that there is a partial replacement of Nat
by K+ as a result of the ion implantation consistent with a simple ion
exchange process:
-SiiO-Na+ + Kt + -Si-0 -K’ + Na+ . (2)

For such a simple reaction, replacement of Nat by K+ in the implantation

region should be 1 : 1. However, the depth profiles suggest that more Na’ is
lost from the implantation zone than can be accounted for by simple ion
exchange. It appears that significant amounts of alkali are removed from the
glass during ion implantation, reducing the number of anionic non-bridging
oxygens in the structure via repolymerization.
It has been demonstrated that ion implantation in alkali silicates can lead to
the production of alkali metal colloids. The alkali colloids can be volatilized by
the ion beam resulting in significant losses of alkali from the glass surface [43].
We speculate that this same mechanism might also explain the accumulation of
potassium at the surface of silica observed by AES. In this case, no non-bridg-
ing oxygens are available for the implanted potassium ions. Therefore, the
reformation of the SiO, network [44,45] accelerates the diffusion of potassium
to the surface, where it can be effectively coordinated by atmospheric oxygen
or water (weathering). The conclusion that this diffusion is faster and more
complete in silica than in sodium trisilicate is supported by the decrease of
potassium in the integrated RBS profile compared to the incident ion current
density measured during the implantation. This depletion can be attributed to
 B.J. Burrow et al. / K-implanted Si, SiO, and Na,O’ 3Si0, 179

the rapid diffusion of potassium to the surface and vaporization by the ion
beam as well.
In conclusion, the combination of the chemical sensitivity and surface
specificity of AES with the quantitative ability and depth selectivity of RBS
leads to a rather complete description of a solid surface, within certain
restrictions. These restrictions, clarified in this work, are summarized: (1)
Because of the differences in sampling volume, some ion milling of the sample
prior to AES analysis is necessary. Consequently, there should be no preferen-
tial sputtering or knock-on effects in the standard material. (2) If ion implanta-
tion is used, a flat profile at some shallow depth should be formed. The
shallow depth minimizes the inevitable atomic mixing that occurs during ion
bombardment and the flat profile provides a region where where the energy
resolution of the RBS detector is not critical. (3) Electron and ion beam
induced artifcats must be minimized. This precludes the use of alkali ions for
such a study at room temperature. (4) Finally, the materials chosen should
ideally be those to which RBS and AES are most sensitive. This requires high
mass atoms for ion scattering and atoms which have high Auger sensitivities.

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