Crater Edge Profiling of Ni/Cr Sandwich

Multilayer Thin Films by Scanning Auger

Microscopy (SAM)

A. Zalar
Institute for Electronics and Vacuum Techniques, Teslova 30, Yu-6001 Ljubljana, Yugoslavia
S. Hofmann
Max Planck Institut fur Metallforschung, Institut fur Werkstoffwissenschaften, Seestrasse 92, D-7000 Stuttgart 1, FRG

The principle of the technique of crater edge profiling is described as an alternative method to conventional
sputter profiling. The predictions for the lateral composition profile assuminga Gaussian intensity distributionof
the primary ion beam are tested for a multilayer sandwich structure of Ni/Cr layers of 11.5 nm single layer
thicknesses after Ar+ ion sputtering through 20 layers and scanning Auger microscopy with a 10 p m diameter
electron beam. Due to the small angle of 442” of the slope of the crater formed by ion sputtering, a magnification
factor (lateral variation/depth variation) of 5 x lo3is obtained.

INTRODUCTION distribution, it can be checked whether the condition

In depth profiling by AES combined with argon ion
bombardment,”2 a flat-bottomed crater within the
analysed area is of decisive importance with respect to
optimum depth resolution44 This condition requires a
beam of primary ions with uniform intensity over this
area. Any deviation from uniformity will cause a
degradation of the depth resolution.’-8 A still unsolved
problem is the determination of the magnitude of this
instrumental effect of ion beam inhomogeneity
compared to that of the other effects which contribute to
a limited depth resolution, such as: Auger electron
escape depth, original surface roughness, crystal orien-
tation and defects, sputtering induced surface roughen-
ing, ion mixing, preferential sputtering, surface and bulk
diffusion e t ~ . ~ ’ ~
With the exception of orientation effects, the relative
depth resolution Az/z defined by the broadening Az of
~ - ~ the sputtered depth z ,
a rectangular p r ~ f i l e ~ ’upon
generally decreases with because the absolute
contribution is either independent of depth (Az/z z - )
or increases with the square root of the depth
(Az/z oc 2-l”). However, the relative depth resolution
caused by primary ion beam inhomogeneity, AzI/z, is
constant because AzI is ro ortional to the primary ion
flux and therefore to z.’~ &r this reason, AzI becomes
the limiting contribution to the total depth resolution for
large z. With respect to the order of magnitude of
measured Az value^,^ AzI/z G lo-’ can be tolerated up
to a sputtered depth z of about 100nm. For larger
depths (up to 1 p m or beyond) AzI/z should be at least
one order of magnitude lower, i.e. SW3.This value
corresponds to the required ion beam homogeneity. It is
usually met by rastering a focussed ion beam over a large
With a static ion beam, and knowledge of the electron
beam diameter and the shape of the ion current density
ccc-0142-2421/80/0002-0183
@ Heyden & Son Ltd, 1980
AzI/z s is met. Assuming a Gaussian ion intensity
profile, resulting in z ( x ) = zo exp (-x2/2v2)
the opti-
mum case is an Auger analysis at the centre (Fig. 1,
electron beam at A). If dI is the FWHM (‘diameter’) of
the primary ion beam and d, that of the electron beam, a
simple calculation gives approximately:
where x is the lateral shift of the electron beam from the
maximum intensity (centre) of the ion beam. For exam-
ple, d I= 2 mm and x = 0.5 mm give AzI/z = 5% for a
100 p m electron beam diameter, whereas AzI/z < 1%
is obtained for a mismatch x s 2 mm with an electron
beam diameter of only 5 p m . This demonstrates the
advantage of the small electron beam diarileter used in
scanning Auger miscroscopy (SAM).’”” Another
advantage is the applicability of an alternative method to
obtain depth distribution profiles: the so-called crater
edge profiling10”2 first described by Taylor et It is
analogous to the conventional angle-lapping method
used in electron microprobe analysis.
Since a static primary ion beam produces a crater of a
shape which is similar to the ion current density dis-
tribution in the x-y plane, a crater with a more or less
Gaussian profile is generally ~ b t a i n e d If. ~the electron
beam is scanned from the bottom of the crater to the
edge (Fig. l),the depth analysed gradually decreases.
The important difference from the conventional angle-
lapping technique is that the angle with respect to the
original surface can be made several orders of magni-
tude smaller in the crater edge technique.
The following shows how crater edge profiling is
performed and how the slope of the crater can be
evaluated by a multilayer sandwich sample of Ni/Cr of
known layer thickne~ses.’~.’~
$02.00
SURFACE AND INTERFACE ANALYSIS, VOL. 2, NO. 5, 1980 183
 A. ZALAR AND S . HOFMANN

RESULTS

Figure 1 shows the principle. Assuming a Gaussian

shape of the primary ion beam, the cross section of the
crater should have a similar shape. The relation between
the depth scale ( 2 ) and the lateral scale (x) defined by the
movement of the electron beam in the x direction ('line
scan') is given by the slope angle a ;

tan a
az(x)
=--- -Ad (2)
ax Ax
NI Cr NI Cr NI Cr NI
The maximum slope for a Gaussian profile as indicated (b)
in Fig. 1 is given by:
20
tan a, = 0.6 - (3)
X,

where zo is the sputter depth at the centre and x, is the x

value corresponding to the standard deviation u of the
Gaussian function. It is recognized that the slope
remains almost constant around its maximum at x = u.
The deviation is within s 10% of tan a, from x = 0 . 7 ~
to 1 . 3 5 ~(see Fig. 1). In the experimental set up the
angular relationships between the normal to the sample
surface, and the ion and electron beams in the y-z plane
must also be considered. However, in this case they can
be neglected because their directions are perpendicular
to the x axis.
As an example, crater edge profiling was performed
on a multilayer sandwich sample consisting of alternat-
ing Ni and Cr layers of thickness 11.5 nm, which were
evaporated on to an optical polished flat glass sub-
strate.13 The thickness was controlled during evapora-
tion by a quartz microbalance. Sputtering was done with
a static beam of 1keV Ar' ions from a 5 keV gun in a
commercial SAM apparatus (Physical Electronics
Industries-now Perkin Elmer Physical Electronics
Division-Model 545). When the glass surface was
reached in the centre area of the primary ion beam, the
sputtering was stopped. By rastering the 1 0 p m
diameter electron beam over a limited sample area and
NI Cr NI Cr NI Cr Ni
H
100p m
Figure 2. Auger spectroscopicelemental mapping of a section of
the Ni/Cr multilayer structure shown schematically in Fig. 1.
simultaneous observation of the negative peak intensity
of the Cr (529 eV) or the Ni (848 eV) Auger signal, the
elemental maps of these elements were obtained as
shown in Figs. 2(a) and (b).
The striation structure gives a qualitative picture of
the radial elemental distribution with a curvature in the
direction of the centre of the sputtering crater which is
outside the upper left of the figures. The intensity
modulation is difficult to quantify because of the some-
what arbitrary contrast settings and relatively high noise
(dependent on the sweep rate). However, a line scan
performed through the centre of Figs 2 (a) and (b)gives a
more quantitative result of the revealed radial dis-
tribution of the elements.
The line scans for the Ni and Cr signals are depicted in
Fig. 3, which resembles the conventional depth profile of

I
a multilayer s t r ~ c t u r e . With
' ~ the known layer thickness,
h tan a = d
the crater profiling conditions assumed in Fig. 1 can be
Ax
fa
U
L I NI i
Cr I
I
d
NI
b Cr
z
1.0 I I I I
0 0.5 1.0 1.5 2.0
Normalized distance, x / u
Figure 1. Principle of crater edge profiling: normalized crater
depth z/zoas a function of the normalized distance x / u from the
centre if the assumed profile has a Gaussian shape with standard H
100 p m
deviation U. Optimum depth resolution is obtained with an elec-
tron beam at A; B indicates the scanning position used for crater Figure 3. Line scans for the Cr (529 eV) and Ni (848 eV) Auger
edge profiling. a, is the maximum slope angle given by Eqn (3). peak-to-peak height signal across a selected region of the crater
The Ni/Cr multilayer structure profiled is schematically shown. from layers 18 to 10 (see Fig. 5).

184 SURFACE AND INTERFACE ANALYSIS, VOL. 2, NO. 5, 1980 @ Heyden & Son Ltd, 1980
 CRATER EDGE PROFILING OF Ni/Cr SANDWICH MULTILAYER THIN FILMS
x (pm)
Figure 4. Evaluation of the shape of the crater using the position
of the maxima and minima of the Cr and Ni signalsfrom Fig. 3 and
the known single layer thickness, d = 11.5 nm.
checked, as seen in Fig. 4. Here the position of the
maxima and minima of the Cr and Ni signals on the x
axis (Fig. 3) are plotted against a constant layer thick-
ness, giving a picture of the crater edge. A constant slope
is obtained over a wide range.
It should be mentioned that the constant layer thick-
ness applies only if the sputtering rates for both elements
are the same, as is the case for Ar’ sputtering of Cr and
~ i13.14
. From the known scanning display magnification
(250x), the x scale is calibrated, giving an apparent
layer thickness of about 6 0 p m on the x scale. This
corresponds to the ‘real’ 11.5 nm on the z scale. There-
fore, we can calculate the ‘magnification’ factor accord-
ing to Eqn (2)
11.5 x 1 0 - ~
tan a = = 1.93 x lop4
60 x
This means that the angle a is as small as 1.23”x
or 44.3“.
DISCUSSION
The results in Figs 3 and 4 are in agreement with the
predictions following from Fig. 1:whereas tan CY is fairly
constant in the middle regions, the angle CY is smaller at
the left and right hand sides, with deviations in the
expected direction if a Gaussian profile is assumed. This
corresponds to a reasonable primary ion beam diameter
(FWHM = 2.35 a ) of x, = 1.7 mm for zo = 230 nm
according to Eqn. (3).
The increasing peak intensities from left to right (Fig.
3) may be due to an increasing contribution of the
backscattered electrons if the underlying metal layer
becomes thicker. Furthermore, the acceptance of the
analyser may change along the x axis so that a direct
evaluation of the relative peak heights in terms of depth
r e s ~ l u t i o n ~appears
~ ” ~ not to be justified here. The
@ Heyden & Son Ltd, 1980
1 4 . . . .
0 50 100 150
Sputtering tme ts (min)
Figure 5. Conventional AES depth profile of the Ni/Cr multilayer
sample performed with 1 keV Arf ions (from Ref. 13). To be
compared with Fig. 3.
inherent depth resolution of the method is limited by the
primary electron beam diameter with respect to the x
scale, i.e. a diameter of 10 p m corresponds to 1.5 nm in
depth. This is substantially smaller than the depth
resolution expected in the region from the 10th to the
18th layer shown in Figs 3 and 4.
A comparison with Fig. 5, which is a sputtering profile
of a similar layer given in an earlier p ~ b l i c a t i o nshows
’~ a
remarkably good agreement with respect to the shape of
the profile between layers 10 and 18. In this region, the
depth resolution from the sputtering profile was found to
be about l o % , i.e. 14 nm. From the general evaluation
scheme for the profile of a sandwich layer of thickness
d l s it can be estimated that limited plateaus (in a
mathematical sense) instead of the distinct maxima
(recognized in Fig. 3) should occur if A z / d < O S . That
means Az is at least 6 nm as seen from the shape of the
profile, i.e. measured depth resolution is not limited by
instrumental factors but by the various additional
contribution^.^'^.'
CONCLUSION
In the case presented, the crater profile could be checked
by the known layer structure of the sample. Generally,
the primary ion intensity distribution in the x direction
has to be measured, e.g., by a Faraday cup.4tan cy can be
determined from Eqn (2) with z =it. In principle, a
change in the sputtering rate i can be taken into
account. Of course, depth resolution in crater edge
profiling will also depend on the additional Az contri-
butions as discussed elsewhere.5373x
The advantages compared to conventional depth
profiling are:
(a) The depth profile can be obtained at ease after
sputtering with almost no limitation in data acquisition
time over the whole area of the crater. Thus, possible
lateral inhomogeneities of the elemental in depth dis-
tribution can be studied (the question of the ‘typical’
depth profile representative of a sample is of great
importance in practical applications).
(b) In the related technique of spherical erosion by
‘ball rate ring''^^'^ the crater is better defined. However,
SURFACE AND INTERFACE ANALYSIS, VOL. 2, NO. 5, 1980 185
 A. ZALAR AND S. HOFMANN
the absolute depth resolution is rather restricted due
to the mechanical roughening. Compared to sput-
tering, crater formation by ball bearing appears only
useful if a large depth range of several microns is of
interest.
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186 SURFACE AND INTERFACE ANALYSIS, VOL. 2, NO. 5, 1980
The most outstanding feature of crater edge depth
profiling is the possibility of obtaining large lateral
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angle, < 5 ’ ) using conventional ( S 10 k m electron beam
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Received 26 March 1980; accepted 6 June 1980
@ Heyden & Son Ltd, 1980
@ Heyden & Son Ltd, 1980