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Measurement of the roughness of nano-scale surfaces, both unannealed and with limited

anneal, by atomic force microscopy

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2014 Meas. Sci. Technol. 25 105001

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 Measurement Science and Technology

Meas. Sci. Technol. 25 (2014) 105001 (12pp) doi:10.1088/0957-0233/25/10/105001

Measurement of the roughness of nano-scale

surfaces, both unannealed and with limited
anneal, by atomic force microscopy
M P Seah
Analytical Science Division, National Physical Laboratory, Teddington, Middlesex TW11 0LW, UK

E-mail: martin.seah@npl.co.uk

Received 3 December 2013, revised 1 July 2014

Accepted for publication 14 July 2014
Published 29 August 2014

Abstract
The roughness and bias measured for surfaces scanned by a parabolic atomic-force microscope
tip are analyzed computationally for surfaces exhibiting a random, Gaussian population of
heights, uncorrelated from pixel to pixel. The fraction of the surface with which the probe is
in contact is then analyzed in detail to show the area fraction of the surface that is, in practice,
contacted within a defined tolerance. This shows that it is very difficult to measure much of
these surfaces for any significant roughness even though the roughness value may sometimes be
approximately correct. The surface is then allowed a limited anneal, and the improvement in the
validity of the measurement is determined. Annealing removes the very short-range structure
and permits more meaningful roughnesses to be determined with a greater fraction of the
surface contacted by the probe. This limited anneal may simulate the behaviour of hot atoms
that are incident or impacted by energetic ions and that rapidly cool at the surface. Asymmetric,
non-Gaussian height distributions are also analyzed, and these generate a significantly different
measurement bias that can be more sensitive to the tip radius. The height distribution shapes
alter with the tip radius, so accurate estimation of the originating height distribution is not
possible. Simple equations are provided to describe the effects.

Keywords: AFM, atomic force microscopy, depth profiling, roughness, SPM, step heights

(Some figures may appear in colour only in the online journal)

List of symbols and their definitions

D0 pre-exponential coefficient of surface n number of results

diffusion
DS surface diffusion coefficient
G surface diffusion distance given by
equation (6)
G0 distance parameter describing Sq(G,R = 0)
in equation (7)
H tolerance describing the height by which
the tip is allowed to miss any given point
on the surface
j index number for results
k Boltzmann constant
Q activation energy for surface diffusion
R effective radius of the parabolic probe as
defined in equation (3)
Rq root mean square height deviation from the
mean for a single line trace
s standard deviation of the heights of the
original uninterpolated surface points
Sq root mean square height deviation from the
mean for an area of the surface
Sq(G,R) value of Sq as dependent on values of
G and R

0957-0233/14/105001+12$33.00 1 © 2014 Crown copyright  Printed in the UK

Meas. Sci. Technol. 25 (2014) 105001
Sq(G,R = 0) value of Sq as dependent on values of
G at R = 0
Sq(G = 0,R = 0) value of Sq at G = 0 and R = 0
Ssk skewness of the surface height distribution
t elapsed time at temperature for the
annealing
T sample temperature, Kelvin
TM sample melting temperature, Kelvin
x distance in one azimuth in the mean plane
of the sample
y distance in an azimuth orthogonal to the
x-direction in the mean plane of the sample
z distance in the direction orthogonal to the
xy plane of the sample
zj jth result for z
z mean height of a population of heights
α angle of tip axis from average surface normal
δ pitch of the grid on which the original
inde­pendent Gaussian height distribution
is defined
Δ distance parameter describing an effective
pitch arising from annealing in equation (8)
Φ(R,H,G) percentage of points measured for a tip of
radius R, within the tolerance H for a sur-
face with annealing G.
Φ(R,H = 0) percentage of points measured for a tip of
radius R, at zero tolerance H for a surface
without annealing, i.e. G = 0.
Φ(R,H = 0,G) percentage of points measured for a tip of
radius R, at zero-tolerance H for a surface
with annealing G.
σ defining standard deviation of the heights
of the independent Gaussian height distri-
bution at the pitch δ.
1. Introduction
The measurement of the roughness of surfaces at the atomic
and nano scale is important for many engineering, electronic
and device applications. Such measurements may be made
using traditional stylus instruments that have a sub-nanometre
height resolution but, unfortunately, only have a lateral resolu-
tion of the order of 1 μm. In many cases, the surface roughness
can be at the atomic scale both laterally and with height, and
these heights cannot then be accurately measured. The atomic-
force microscope (AFM) allows a more effective operation in
this regime [1, 2], with probes that commonly have a radius of
10 nm and, in exceptional cases, a radius closer to 1 nm with,
say, a carbon nanotube and other terminations.
The use of the AFM thus gives greater fidelity in measuring
finer-scale roughnesses and provides a profile of the measured
surface closer to the true profile. The resultant measures of the
surface roughness and other parameters are then closer to the
true values. However, it is not clear how close the result is to the
required measurement. Some issues were dealt with in detail in
an earlier study [3], upon which the present work builds.
Sub-nanometre and nanometre-scale roughnesses often
occur in wafer production, but there the method of manufacture
2
M P Seah
ensures that the pitch of the roughness is generally not too short,
and reliable data is obtained. However, in forming films by high
vacuum vapour or plasma deposition, short-range roughnesses
may occur. Additionally, in sputtering, for example, the compo-
sition-depth profiling of layered materials using surface anal-
ysis techniques such as Auger electron spectroscopy (AES),
secondary ion mass spectrometry (SIMS) or x-ray photoelec-
tron spectroscopy (XPS), much of the interface resolution or
blurring that limits the depth resolution is attributed to sputter-
induced roughness. There, the roughness is often measured as
the standard deviation of the heights of points on the mean sur-
face plane at any instant during the sputter profiling. It is often
assumed that these heights describe a Gaussian distribution
that, added to other contributions, controls the depth-resolution
[4–7]. Non-Gaussian [8–10] and multiple Gaussian profiles
[11] also occur, and any particular distribution may be ana-
lyzed, as discussed below. At coarser pitches, Greenwood and
Williamson [12] and Whitehouse and Archard [13] show that
the heights and the asperities for grit-blasted surfaces (which, in
the early studies of sputtering, were taken as a useful analogue)
exhibited a Gaussian population of heights in the range of up to
2 or 3 sigma from the mean heights. Of course, in sputtering at
high-ion fluences, other structures can form [14, 15] that are of
significant size, but we shall not consider those here.
The lateral pitch of roughnesses formed in sputtering will
be of the order of the individual sputter crater sizes, which
may well be at the atomic scale for sputtering yields of the
order of unity [16], rising to ~5 nm for yields of ~10 000 for
polymers sputtered by argon clusters [17–19].
In much published work, the roughness, when given
by a single numerical value, is the root mean square devia-
tion (RMSD) of the heights in a transverse profile about the
mean line of a specific sampling length, as described in ISO
4287:2009 [20]. In the present work, we shall assume a mac-
roscopically flat surface of infinite size, and provide calcula-
tions to which no filters are applied. In general the symbol Rq
is applied to the RMSD measure of roughness from a line trace
[20], but here we use Sq, the equivalent measurement for an
area [21]—in the ideal case of uniform roughness, these two
parameters have the same value. The use of the area measure
here is to avoid specific alignments of the surface and tip grids
in the computation discussed later. To assist the reader, a list
of symbols and their definitions is provided.
In any measure of a surface using a mechanical stylus, the
resulting profile is not a convolution of the true profile with
an instrumental-broadening function, but a dilation of the
true profile by the mechanical probe [22–24]. Had the former
been the case, although the roughness would be reduced, the
mean height of the surface would be correctly maintained,
whereas in reality, both the roughness and the mean height
are affected. Some of these issues are discussed in detail in
the earlier work [3] for surfaces exhibiting Gaussian uncor-
related height distributions. A surface with a Gaussian height
distribution but with the variations only occurring over long
spatial wavelengths could be measured with great accuracy,
and it is only as the wavelength of these effects approaches or
falls below the radius of the mechanical probe tip, that major
errors may accumulate.
Meas. Sci. Technol. 25 (2014) 105001
The surfaces and films studied for many device applica-
tions and subsequently profiled as above exhibit few long-
wavelength contributions to roughness, so analysts will profile
areas with side dimensions that range from submicrometre to
greater than a millimetre without observing or expecting any
increase in roughness. Many examples exist in the literature of
surfaces that are described by self-affine fractals [25], which
are important in contact mechanics and other areas [26]. In
these, a Fourier transform of the surface profile shows a power
spectrum with an increasing amplitude and reducing spatial
frequency (increasing wavelength). Rq then increases with
the profile scan length and can be proportional to that length.
Such samples, in which the Rq is dominated by the longer
wavelength contributions, are not covered in the present work.
In the literature, the reader will find many profiles described
with Gaussian or similar height distributions that include the
adjective ‘random’. The random aspect of the height distribu-
tions also incorporates a de-randomising effect by including
a correlation between local heights that would effectively
reduce the amplitude of the high-frequency elements in the
line profile [27–30]. The use of Fourier transforms and cor-
relation lengths are popular in optics, as well as in studying
surfaces where periodic effects also occur, such as some
mechanical machining. Here, we have no periodic effects and
shall work in real space to maintain transparency in the effects
observed. We shall start with no correlation length in the data.
For calibrating stylus and AFM instruments for their height
measurement and roughness, step height and sinusoidal cali-
bration standards are available. In interlaboratory tests, these
show that nanometre uncertainties may be achieved for rough-
nesses in excess of 100 nm [31–34]. These standards are effec-
tive, and it is assumed in the present work that such calibration
has been completed.
In the present work, we shall calculate the roughness of the
surface using the measure Sq for a surface area, Sq being the
root mean square of the height distribution for a large number
of measurement points set in the usual square digital grid or
array. We shall also calculate the mean height of the surface,
since this is important for measuring film thicknesses in which
the deposited film has a different roughness from that of the
substrate. This aspect is largely covered in the earlier study
[3]. In that study, both flat- and ball-ended probes were used,
but here we shall use a paraboloid probe with a tip generated
by rotation of a parabolic profile, since this gives results that
may be scaled with the original roughness. This was not pos-
sible with the ball-ended probe, and led to additional com-
plexity in following the effects of the different variables.
We also consider the effect of a limited anneal of the
Gaussian uncorrelated height distributions in our square array
so that the heights of the array points slowly become more cor-
related with time. Annealing is usually considered for high-
temperature studies, but here we are concerned with very
small-scale movements that may result from an incident hot
atom or surface atom impacted by an energetic ion, which is, in
effect, a limited anneal occurring during the surface generation.
This is covered in the next section. Additionally, we consider in
detail the number of surface pixels (area fraction of the surface)
in the array that are either exactly measured or measured within
3
M P Seah
defined tolerances, as a function of the scanning-tip radius.
These parameters are important as they give a better sense, in
general, of the validity of measurements. Using a given model
of the surface, we may find that measures such as roughness
are or are not weakly affected. But if we know that only half or
less of the surface points are accurately measured, any deduc-
tion about the remaining part may only be an informed guess,
even if the measured value of the roughness seems correct. This
arises since any point not actually contacted in the dilation pro-
cess of the tip scanning the surface is at some unknown height
below that measured. The model of the surface being used may
or may not be a good description, but the degree of unknowing-
ness must always be a significant aspect of the uncertainty that
should be associated with measures such as roughness. This
unknowingness is omitted in uncertainty statements that are
usually based simply on the accuracy of the calibration of the
x-, y- and z-axes and the repeatability standard deviation of the
roughness values provided by the instrument software.
The surfaces that we model are isotropic, amorphous,
incompressible solids scanned by isotropic, amorphous,
incompressible AFM tips.
2.  Limited annealing and surface diffusion
Surfaces do anneal at ambient temperatures or, locally, during
the thermal spike of the arriving or departing atoms during
surface generation, and the extent to which this occurs is, for
many elements, related to the melting temperature, TM. The
action of temperature is to allow atoms to move by one or more
displacement mechanisms either through the bulk, by bulk dif-
fusion, or across the surface by surface diffusion. This atomic
movement has a random element but, at surfaces, there is a
net drift of material driven by the reduction in surface energy
to reduce the surface roughness. At low temperatures the sur-
face diffusion is the dominant displacement mechanism. We
shall not consider any of the higher-temperature mechanisms.
The root mean square displacement of the distances moved in
time, t, is (2DSt)0.5, where DS is the surface diffusivity [34–
36]. It is sometimes clear when studying sample roughnesses
by AFM that the surface being studied has rearranged between
the instant at which characterization is required and the time
of analysis [8], although quick working may sometimes be
sufficient to overcome this.
For many of the metallic and semiconductor surfaces it is
assumed that the surfaces are fully stable, but that assumption
may or may not be true for the surface under study. Additionally,
roughness measurements are becoming increasingly important
for organic materials used in devices and display technology.
These are closer to their melting points at ambient temperature.
Exposure of a sputtered or deposited surface away from the
environment in which it is created and to the ambient environ-
ment for AFM study may cause, say, an oxide film to form or
for adventitious hydrocarbons to be adsorbed [37]. Either of
these mechanisms may well help stabilize the surface, but they
may also have changed the surface topography if the original
topography should have been measured. Furthermore, adsorp-
tion of water on a hydrophilic substrate may cause de-wetting
or break-up of any thin-film overlayer.
Meas. Sci. Technol. 25 (2014) 105001
Figure 1.  Conditions for a root mean square surface diffusion of atoms over 1 nm, 10 nm and 100 nm, (a) as a function of the sample
melting temperature from equation (1) and (b) as a function of the activation energy Q for surface diffusion from equation (2).
The effects of surface atomic diffusion may be calculated from
the assessment of surface diffusion coefficients by Seebauer and
Allen [38], in which, for low temperatures, two equations  are
provided that give very similar results. The average of these
gives, for DS at temperature, T, the empirical relation
DS = 0.037exp(−6.77TM / T ) cm2/s.
(1)
From this, one may deduce the time for atoms to diffuse
1 nm, 10 nm and 100 nm across the surface at 300 K, as shown
in figure  1(a), for typical values of TM ranging from 800 K
to 2000 K, i.e. Al or Sb on the left of the plot to Ti or Pt on
the right. The ordinal scale ranges from 0.1 s (very fast) to
4 months. We see that significant atomic diffusion may occur
for many materials over the time scales for AFM measure-
ment. An alternative equation may be used from the compila-
tion of Antczak and Ehrlich [36]:
DS = D0 exp(−Q / kT ) cm2/s.
(2)
Here, k is the Boltzmann constant, D0 is typically 0.001 cm2/s
and Q, the activation energy for surface diffusion, ranges from
0.4 eV to 1.0 eV per atom. This range can occur for one metal
for displacements on different crystal faces. (In the present
work we restrict ourselves to amorphous materials.) The cor-
responding plot at 300 K is shown in figure  1(b). Although
equations  (1) and (2) are for atomic diffusion and have not
necessarily been evaluated for organic materials, it is clear that
their low TM values could offset any slowness in molecular
diffusion associated with their often-interlocking molecular
structures. In practice, for many elements these movements
may be inhibited by surface oxidation or contamination.
However, for the organics, which do not necessarily suffer
from these issues, these plots may apply directly.
It is clear that some surfaces will retain their full roughness
as formed, whilst others may anneal to a limited extent that
may not be obvious in a cursory examination.
3.  Analysis of the measured roughness and bias of
Gaussian height distributions
3.1.  The surface and the probe
The surface analyzed here is based on the surface used pre-
viously [3]. Briefly, this surface consists of a grid of points
4
M P Seah
at spacing δ, in which the heights at each point are uncorre-
lated, and with a Gaussian population of heights with a stan-
dard deviation, σ. This could represent a vapour deposited or a
sputtered surface maintained at low temperature. In this case,
δ could be as low as 0.25 nm for elemental condensates or as
high as 5 nm for very large molecular condensates. In terms
of the roughness formed during sputtering, the lower δ value
is unlikely. The scanning probe tip will also be described by
its surface based on the same grid separation, δ, but since the
two grids need not be in registry, the description of the surface
between the original grid of points also needs consideration.
We generate these intermediate points on a surface within each
square formed by the original grid points by linear interpo-
lation, first along the inter-point edges in the y-direction, and
then in the x-direction between those respective interpola-
tion points. This forms a doubly ruled, hyperbolic paraboloid
joining surface that is never higher than the highest corner point
or lower than the lowest corner point. (The interested reader
can see many example images of such surfaces by entering
‘hyperbolic paraboloid’ into an internet search engine, so a
figure is not included here.) On this joining surface, we may
devise sub-grids with pitches of δ/2, δ/4, δ/8, etc. The subgrid
at δ/4 was found [3] to give similar results to finer grids but
is less demanding computationally, so is used here. This new
sub-grid has a population of heights that is close to Gaussian
with a standard deviation that is less than σ and, for the present
interpolation, reduced to 0.659σ. A two-dimensional spline
function could be a better joining surface, but is much more
computationally intensive and leads to the same general results
except, as discussed below, when R is very small.
The geometries of the probes used previously [3] were
flat-ended and ball or hemispherically ended. The flat-ended
probe had the advantage of providing results that scaled with
σ, so providing more homogenized data. However, the flat-
ended probe is not a good approximation to the AFM probe
tip. With the more realistic ball-ended probe, this scaling does
not occur, and computations were required for many radii and
σ values. In the present work, we use a parabolic probe that
has the advantages of both of the previous probes since the
results scale with σ, but the end of the probe is also nearly
spherical and may more accurately describe probes used in
practice. Figure 2 shows a ball-ended probe and the shape of
the parabolic probe described by
Meas. Sci. Technol. 25 (2014) 105001
Figure 2.  Shape of the ball-ended probe used in [3] and the
matching paraboloid end used here.
x 2 + y2
z =
(3) ,
2R
where R is the radius of the sphere that matches the end of
the parabolic probe accurately to a distance x = 2R/3 from the
probe axis. All points referring to the tip on its sub-grid are
described by equation (3) and not by the doubly ruled joining
surface.
In practice, with AFMs, the axis of the probe is tilted at
an angle, α, in the range 5°–12°, with respect to the average
surface normal. This will have little effect whilst the contact
points are in the range −0.5 ≤ x / R ≤ 0.5 but, beyond that,
the fidelity of measurements degrade even more rapidly than
shown here. We shall not consider the added complexity of
α. In practice, tips also wear, so that R increases as the tip
becomes flattened. This is especially true for the sharpest tips.
This will not be considered separately, but the effect of R is
considered. The analyses presented here are thus for optimal
cases that may or may not be achieved in practice.
3.2.  Roughness and bias measured with the paraboloid
In the present calculations, the tip is set vertically and scanned
across the surface, and the height and RMSD values of the
heights of the tip are calculated for positions on the grid of
points at separation δ, as well as the 15 interpolated points at
separation δ/4 in the sub-grid. The general appearance of the
surface, the dilation by the tip and the resulting populations of
heights for the flat-ended and ball-ended probes are detailed
in the earlier study [3], and will not be presented again here.
However, the results for the bias and Sq as a function of the
parameter R do change a little, and are shown in figure 3. This
differs from the results previously shown since the scaling
with σ allows the use of the reduced abscissa of Rσ/δ2 instead
of R/δ, there being one curve for all σ/δ values, and the data
is all for the interpolated surface. These results are important
for correcting film thickness measurements using a step edge
of the film, where the film and substrate have differing rough-
nesses, as described earlier [3].
At the start, the surface has a Gaussian distribution of
heights. The population after scanning is still closely Gaussian
5
M P Seah
Figure 3.  The mean height and roughness for the interpolated,
Gaussian height distribution surface measured with the parabolic
probe.
but, as before [3], there is a very small excess of the higher
points that is only noticeable when many points are measured.
The exact results here and elsewhere in this study depend,
of course, on the distribution of heights, and the mean height
towards the right in figure 3 will be sensitive to the few points
in the tail of the distribution at high heights. Additionally, the
exact results towards the left depend on the precise form of
the interpolated surface between points. However, the gen-
eral behaviour shown in figure 3 is relatively robust to these
parameters.
3.3.  Surface points measured correctly
In the previous study [3], we noted that the number of sur-
face points contacted by the probe to give the correct height
rapidly reduced as the tip radius increased. The data there
depended on σ/δ, but now the situation is simplified, as shown
in figure 4. Here, the grid for defining the tip geometry aligns
with the grid or sub-grid of points interpolated at δ/4 that
define the surface. If the grid for the tip is shifted laterally
a small fraction of δ away from the surface grid, the surface
is detected less frequently since any surface maxima are on
the surface grid points, and the dilated region very close to
that maximum will be the top of the parabola describing the
inverted tip. Exactly what occurs depends on details of the
shape of the interpolation surface, but we shall see later that
these details are unimportant if R > δ. For the contacting of
surface points by the apex of the tip, for the doubly ruled
joining surface described, only ~1/5 of the surface points
may be contacted at these infinitesimal sub-divisions of the
sub-grid. These points are all local asperities. This is a rather
severe constraint afforded by the doubly ruled surface that
would not be the case for a spline connecting surface. We
therefore calculate the percentage of times, Φ(R,H = 0), the
apex point makes contact with surface points when the tip
of radius R addresses each point in the grid or sub-grid just
interpolated to δ/4.
Figure 4 thus shows how the tip only sees 90% of the
points at
Rσ / δ 2 ≤ 0.06
(4)
Meas. Sci. Technol. 25 (2014) 105001
Figure 4.  Percent of surface points measured correctly as a function
of Rσ/δ2. The grid for the tip aligns with the interpolated sub-grid of
surface points.
Figure 5.  Percent of surface points measured within the
tolerance ±H a function of Rσ/δ2 for values of H/σ increasing from
0 to 0.5 at intervals of 0.05.
or, since the true roughness of this surface, Sq, is 0.659σ,
RSq < 0.04δ2. Equivalently, this means δ > 5(RSq)0.5 describes
the minimum pitch of the roughness to see 90% of the points.
Equation (4) may also be derived using the probability model
discussed in reference [3]. The value of 0.06 on the right-hand
side of equation  (4) is affected by the precise shape of the
joining surface, but is a good typical value. The difference in
Rσ/δ2 value between this result for the 16 times more dense
interpolated sub-grid and the result for the original grid at
Φ(R,H = 0) = 50 % is about 3%, and is not significant. If R and
Sq are each 1 nm, then δ > 5 nm, which is significantly greater
than the atomic scale but just within the range 0.25–5 nm of
likely studies. If δ = 5 nm and with R as small as 4 nm, Sq
would have to be less than 0.25 nm to see 90% of the points. It
is clear that, in general studies, only a few surface points will
be contacted. For accepting only 50% of the points, the above
limit only increases by a factor of 2.
In general, analysts wish to study Sq roughness values of
1–10 nm with such tips, and the real situation may not be as
grave as figure 4 since, although the apex may not contact the
surface, it may well be sufficiently close (although not in con-
tact) for there not to be a significant problem. Figure 5 repeats
6
M P Seah
figure 4, but allowing for a tolerance, H, in missing the points
up to H = 0.5σ, i.e. the data shows the percentage of points
measured within a tolerance interval ±H, Φ(R,H). The tip now
sees 90% of the points within the tolerance H if
(Rσ / δ 2 )2 ≤ (0.06)2 + (0.32 H )2,
(5)
so that R does increase with H but, unfortunately, not dra-
matically. To double the limit of Rσ requires H = 0.3, i.e. the
tolerance must reach very wide limits to improve the limit
significantly, but that tolerance is too great for a meaningful
measure. A value of H = 0.1σ would seem to be the limit
of acceptability and, at that level, the improvement is not
significant.
As shown in figure  3, it is fortunate that the measure of
roughness is only weakly affected by increasing R, despite
the lack of contact to most of the surface points and, hence,
meaningful measurements appear to be possible if the rough-
ness is genuinely Gaussian. We shall return to this issue later.
One fortuitously has a good measure, even though much of
the surface is not seen. In the situation of real surfaces, the
randomness may not be maintained at such short range and
indeed, to retain such surfaces, from figure 1(a) they may need
to be kept at a low homologous temperature, say, T/TM < 0.15.
In the next section, we analyze the changes that occur as our
original surface is given a limited anneal either during or after
generation.
Probe tip reconstruction [22–24] and image erosion [39,
40] are important for studying features by AFM, but here, if
the surface points are not contacted, the user can never have
genuine knowledge of their depth below the apparent height
unless informed by other, separate data. Image erosion may or
may not help inform that issue.
3.4.  A limited anneal of surfaces
Here we assume that our isotropic solid has an isotropic
surface energy and diffusion constant. The surface that we
have used so far may be slightly modified in its formation by
the hopping of the incoming atoms a few atomic distances
before freezing, or by the formation of local thermal spikes
during sputtering. This may be modelled as a limited anneal
of the original interpolated surface. We thus convolve that
surface with a two-dimensional Gaussian smoothing func-
tion that describes the surface diffusion. The width of the
smoothing function is defined by a G value equal to its full
width at half maximum (FWHM). The distance of the char-
acteristic diffusion, with a surface diffusivity DS and a time t,
is given by (2DSt)0.5, where:
G2
2DSt =
(6) ,
8 ln 2
i.e. G2 is proportional to the time of diffusion. In figure 6(a)
are shown four line traces for part of the central pixel row
in which the surface is annealed with G = 0δ, 1δ, 2δ and 3δ.
Figure 6(b) shows a plan view of part of the original surface
with G = 0δ. This shows why the lines for G = 1δ, 2δ and 3δ in
figure 6(a) are not simply increasingly smoothed versions of
the line for G = 0δ. Minima for G = 0δ may be swamped in the
Meas. Sci. Technol. 25 (2014) 105001 M P Seah

Figure 6.  The Gaussian annealed interpolated surfaces with G = 0δ, 1δ, 2δ and 3δ, (a) line traces for the interpolated surfaces along the
central grid row, (b) plan view either side of the left-hand end of the central grid row in (a) for G = 0δ, and (c) histograms of heights with
Gaussian fits. In (a) and (c), the colour scheme is black for G = 0δ, red for G = 1δ, green for G = 2δ and blue for G = 3δ. In (a), the trace for
G = 0δ is the same as that for reference [3], except the start of the trace is further to the right to avoid any end effects. The traces for non-
zero values of G are not simply the trace for G = 0δ smoothed as the data in the orthogonal direction, shown in (b), contribute.

Figure 7. (a) Sq(G,R = 0) for the random interpolated surface at R = 0δ as a function of G and (b) Sq(G,R) before and after anneals with
G = δ, 2δ and 3δ, as a function of Rσ/δ2 for the parabolic probe. The curves are the empirical description of equation (11).

Gaussian smoothing of the anneal by the effects of maxima in Sq (G = 0, R = 0) G 0

the adjacent traces.
Figure 6(c) shows that the histogram of heights remains
fully Gaussian. The standard deviation of the heights
will reduce as G−1 at high G values since the number of
pixels smoothed depends on G2. At small G values, the
method of interpolation effectively places a smooth over
the area of δ2, so there is an effective smooth even at G =
0, which we shall call G0 (although this is not actually a
Gaussian smooth). The value of Sq(G,R = 0) is thus given
approximately by
Sq(G , R = 0) =
(7) ,
(G02 + G2)0.5
where Sq(G = 0,R = 0) is the roughness of the original inter-
polated surface, 0.659σ. Figure  7(a) shows how Sq(G,R
= 0) falls as G increases together with the plot for equa-
tion (7). Figure 7(b) shows how Sq(G,R) further falls as the
R value of the parabolic probe increases. The effect of R,
as G increases, becomes weaker and weaker since the sur-
face progressively loses its very short-range structure in the
annealing.

7
Meas. Sci. Technol. 25 (2014) 105001
Figure 8.  The mean height normalized to Sq(G,R = 0) as a function
2
of Rσ/δ for the original interpolated and annealed surfaces. The
curves are the empirical description of equation (10).
Figure 9.  The percent of surface points measured correctly as a
function of Rσ/δ2 for the interpolated and annealed surfaces. The
curves are the empirical description of equation (12).
It is useful to introduce the parameter Δ given by
⎛ G 2 + G2 ⎞0.5
Δ = ⎜ 0 2 ⎟ δ,
(8)
⎝ G0 ⎠ (11)
so that
Sq ( G , R = 0) / δ = Sq ( G = 0, R = 0) / Δ,
(9)
i.e. it appears as though the behaviour is similar to that of the
unannealed surface if the pitch δ is replaced by a new pitch Δ
given by equation (8).
The effect of annealing on the bias or mean height meas-
ured is also strong. Instead of normalizing against σ, we nor-
malize against Sq(G,R = 0) since that is the measure of the
standard deviation of the heights of the annealed surface being
studied. This is shown in figure 8. As with Sq(G,R), the effect
of R is significantly weakened for the annealed surfaces.
The effect of annealing, which reduces the effect of R, is
important and means that practical measurements of such sur-
faces are more faithful. This is shown clearly in the results
for the percentage of surface points measured correctly, as
shown in figure 9. The rather rapid fall seen in figure 4 is now
weakened, and we see for G = 3δ, that 50% of the points are
8
M P Seah
2
contacted up to just above Rσ/δ . However, if the abscissa is
replaced by a possibly more meaningful RSq(G,R = 0)/δ2, then
the 50% point for G = 3δ, instead of appearing at 10 times
the abscissa value for G = 0δ, only appears at 3 times that
value, i.e. there is marked improvement in the validity of the
measure of Sq for the surface on annealing, but part of that
improvement is simply from the roughness being reduced, and
part from the removal of the high-frequency elements of the
roughness.
It is useful to have empirical analytical descriptions of these
behaviours so that parameters may be related or extended. We
do this in the next section.
3.5.  Empirical relationships
We start with the bias or mean height of the surface, as mea-
sured. Previously, the mean height for ball-ended probes was
a complicated function of R and σ. Here, we find for the data
in figure 8:
mean height 4.445 R Sq(G , R = 0)
(10) = 2 ,
Sq(G , R = 0) G 0 + G2 + 0.5 Gδ + Rσ
where G0 = 1.13δ. Equations (7) and (10) describe the solid
curves in figure  8, rather than there simply being curves
joining the data points. For G = 0δ, these results are similar
to, but simpler than, the results for the balled-ended probe dis-
cussed earlier [3].
As before, data in the plot of figure 8 becomes more homo-
geneous if the abscissa Rσ/δ2 is replaced by Rσ/Δ2, confirming
that the pitch is again approximately replaced by Δ. As before,
the population of heights is Gaussian, with a very small excess
for higher points.
Next, we consider the measured roughness Sq(G,R) shown
in figure 7(b). Here we find:
Sq(G, R ) 0.8
= ,
σ ⎡ 2 0.75⎤
0.5
⎣G 0 / δ + G / δ + 0.65G / δ + (0.4Rσ / δ ) ⎦
2 2 2 2

which also gives the solid curves in figure 7(b) as well as for
R = 0δ, in figure  7(a). Note that the effects of G and R are
both to smooth the measured surface, but each operates in
quite a different way. The Gaussian annealing parameter G
is convolved with the original surface, and so acts to smooth
it in exactly the same way as smoothing reduces signal
noise. The number of points smoothed increases as G2, and
so the smoothing, at large G, gives an Sq(G,R) value that is
inversely proportional to G. The probe R value, however, is
involved in the dilation of the surface, which forms an enve-
lope that smooths in the sense that fine local detail is lost,
but the heights of the top-most peaks remain unchanged and
R only weakly affects Sq(G,R). As before, data in the plot of
figure 7(b) become more homogeneous if the abscissa Rσ/δ2
is replaced by RSq(G,R = 0)/Δ2, confirming that the pitch is
again effectively replaced by Δ.
Finally, we consider the percentage of points measured
correctly, Φ(R,H = 0,G), for the interpolated surface. Here:
Meas. Sci. Technol. 25 (2014) 105001 M P Seah

Figure 10.  Data from equation (15) as a function of the tolerance interval and the annealing parameter G, (a) the increase in radius that
may be used to see 90% of the surface points and (b) the percentage of the surface points for Rσ/δ2 = 16.

100 H, for G = 0δ, δ, 2δ and 3δ. Note that the ordinate here is a log
Φ(R, H = 0, G ) = .
⎧ ⎡ 1.66 ⎤−3⎫
1/3 scale. As G increases, H has a more significant effect than it
⎨1 + ⎢0.014
⎩ ⎣ ( (1 + G2 / δ 2 )
(Rσ / δ 2 ) ) ⎥⎦ ⎬
⎭
did for G = 0.
If we consider a very high resolution probe, with R = 1 nm

(12) and δ = 0.25 nm, then Rσ/δ2 = 16σ if σ is in nm. If σ is 1 nm,
Equation (12) is shown by the solid curves in figure 9. then Rσ/δ2 = 16 and, even for this sharp probe, we rarely con-
For a reasonably faithful description of a surface, Φ(R,H,G) tact 90% of the surface points for reasonable tolerance levels.
should be greater than 90%, and equation (12) then provides a In figure 10(b), for Rσ/δ2 = 16, Φ(R,H,G) is plotted versus the
relation between R, σ and G for a given value of δ. Thus, acceptable tolerance, H. This shows that we need G = 3δ and
H/σ > 0.28 to achieve 90% of the surface points to be mean-
RSq(G = 0, R = 0) [1 + (G / δ )2] ingfully recorded.
(13) ≤ , Thus, for these rough surfaces—although, as shown in
δ2 24
figure 7, reasonable Sq(G,R) values are obtained—these meas-
or approximately urements rely on a description from a small fraction of the
Rσ / Δ2 ≤ 0.06.
(14) surface points. The remainder of the points may be modelled
by some estimated height distribution function, as here, but
This is similar to equation  (4). For G = 3δ, the limit on Rσ the evidence for any given valid function is, in practice, dif-
has now increased 10-fold, i.e. if δ = 5 nm, Δ = 16 nm and R = ficult to obtain, and it may be that, for particular experimental
4 nm, then σ < 2.5 nm to see 90% of the surface points, i.e. the data, a very different height distribution function may be
limit is 10 times higher than in the pre-annealed state. Even more appropriate. That the measured distribution of heights is
so, in general, significantly less than 90% of the surface is Gaussian simply tells us that the response of the dilation to the
contacted. highest points is nearly Gaussian and that, whilst appearing
If we wish to incorporate the effect of the tolerance to generate a reasonable estimation of the original surface
interval ±H over which the description is valid, equation (12) roughness, does leave much unknown about the true surface
requires extension with extra terms involving H. The extended that should be incorporated into any stated uncertainty. The
result for Φ(R,H,G) within the interval  ±H is given for assumption of an underlying Gaussian population may be
Rσ/δ2 < 5 and H < 0.5 to better than 3% by quite incorrect, particularly for the important asperities, and
Φ(R, H , G ) the significance of this is discussed below.
100
=
⎧ −3⎫1/3
⎡ ⎛ 1 + G2 / δ2 ⎡ ⎤ ⎞1.66 ⎤
⎪ ⎢ ⎜( { } ⎟ ⎥ ⎪
0.63
1 + ⎢(23.5 − 20H / σ )(Rσ / δ2) − 1.5⎥H / σ
⎣ ⎦
⎨1 + ⎢0.014 ⎬
)
4.  Non-Gaussian height distributions
⎪ ⎜ ⎟ ⎥ ⎪
⎢⎣ ⎠ ⎥⎦
2
⎝
(Rσ / δ )
⎩ ⎭
 It is important to consider whether asymmetry in the height
(15)
distribution affects any of the above conclusions. To skew the
This reduces to equation (12) for H = 0. The general effects height distribution in a systematic manner, we now consider the
of G and R work in opposition, as shown in figure 9, with the original surface and increase the heights of those points above
increasing interval, H, enabling a higher percentage of cor- the median line progressively with their height, and decrease
rectly (within H) measured surface points. those below the median line progressively with their depth, or
From equation (15), we may set Φ(R,H,G) to, say, 90, as vice versa. This leads to an asymmetric distribution with a skew-
shown in figure 10(a). Here Rσ/δ2 is plotted versus the interval, ness Ssk [18, 19] that can be adjusted positively or negatively.

9
Meas. Sci. Technol. 25 (2014) 105001 M P Seah

Figure 11.  The mean height and roughness for the interpolated
surface measured with the parabolic probe, normalized to Sq(G = 0,
R = 0) instead of σ, for Ssk = −1, 0 and +1.

The skewness, Ssk, is defined by the Fisher–Pearson stand-

ardized moment coefficient
n ⎛ z − z ⎞3
Ssk =
(16) ∑⎜⎝ j ⎟⎠
(n − 1)(n − 2) s j

where n is the number of measurements, s is their standard

deviation and z is the mean height of these measurements.
For Ssk values of –1, 0 and +1, without any annealing, the
mean heights or biases of the measured surface as a func-
tion of tip radius are given in figure 11. Also shown are the
measured roughnesses. With the positively skewed surface,
the increased elevation of the uppermost points increases
the magnitude of the bias and vice versa. The change
between Ssk values of –1 and +1 is more than a factor of
2, indicating that unless the originating distribution is well
known, correcting for the bias is uncertain. The effects on
Sq are more marked since, at Ssk = −1, the deeper points are
not seen, and so their strong contribution to Sq(G = 0, R =
0) is ­rapidly lost and Sq is quickly reduced in magnitude.
At Ssk = +1, the distribution of the higher points, which
dominate the profile as R increases, has a strong contribu-
tion to Sq(G = 0, R = 0) and leads to no significant reduction
in Sq as R increases. Figure 12.  Distributions for the three surfaces for Rσ/δ2 = 0, 1
and 5. The distributions for Rσ/δ2 = 0 (the red curves) are for
It is also useful to consider the measured distribution of infinitely high populations, whereas the remainder are for 3,246
heights, and these are shown in figure  12 for Rσ/δ2 = 0, 1 points to indicate a common level of statistical scatter in data.
and 5 for the surfaces with Ssk = −1, 0 and +1. At Ssk = −1, The smooth green-and-blue curves are the fits of Gaussians to
the distribution narrows, as indicated in figure  11, and the emphasize the smallness of the visible asymmetry, although the
skewness also sharply reduces. At Rσ/δ2 = 1, this distribu- Ssk values for Rσ/δ2 = 1 and 5 are 0.1 and 0.3 in (a), 0.5 and 0.4 in
(b) and 0.7 and 0.4 in (c), respectively.
tion is effectively Gaussian, and so the analyst can have no
idea at this stage of the shape of the original height distribu-
tion, or very accurately, of the true value of Sq. At Ssk = 0, which regime is possible but requires the sharpest tips unless
the Gaussian height distribution narrows more slowly and the effective value of δ is significantly higher than used ear-
exhibits an increasingly positive skewness, as noted in sec- lier. With surfaces exhibiting features at many scale lengths,
tion 2.2. At Ssk = +1, the skewness is reduced but still persists skewness may be clearly observed. Stoic et al [41] show such
as Rσ/δ2 increases. At the highest Rσ/δ2 values evaluated here, a distribution for dried cast polymer films where the skewness
the final skewness for all surfaces is very similar, although the appears to arise from distinct surface protrusions.
underlying Sq values are significantly different. Thus, it is very Note that the shape of the distribution is not defined
difficult to deduce much of significance about the intrinsic uniquely by the skewness, and for other shapes of distribu-
height distributions from the measured height distribution tion, the results shown in figures 11 and 12 may or may not be
unless Rσ/δ2  <  0.06, as described earlier in equation  (14), representative. What both show clearly is the marked change

10
Meas. Sci. Technol. 25 (2014) 105001
in the distribution that may occur compared with Gaussian
height distributions.
It is worth noting in figure 12 the numbers of points accu-
rately measured, and for Rσ/δ2 = 1 with Ssk = −1, 0 and +1,
these are only 10, 5 and 4 out of the first 1,500 points. These
points have average heights of 0.56σ, 0.93σ and 1.51σ. The
numbers of points accurately measured are very small and
represent points nearly always above the median line. Most
of the measured points are dilated points from the top part of
the distribution.
5. Conclusions
Gaussian randomly rough surfaces have been analyzed for
measurements by AFM to describe how the measured rough-
ness and apparent height of the surface are affected by scan-
ning with a parabolic-tipped probe. The behaviour is similar to
that found in the previous study [3] using a ball-ended probe,
but here we also include the diffusional effects of a limited,
adventitious surface annealing. This shows that the bias and Sq
values observed as annealing develops are much the same as
for the calculations for the unannealed surface if the original
pitch δ is replaced by a new pitch Δ that is governed by the dif-
fusional distance. We also show that few of the surface points
can actually be measured in practice, even within usable toler-
ances, unless the surface is smoothed by annealing or some
equivalent process. It is the dilation process of the scanning tip
that causes many points on the surface to be unseen. Had the
process involved convolution instead, this would not have been
the case. Height distribution deductions are therefore generally
based on the data from only a few surface points sampled. For
a Gaussian surface, the measure of Sq is only weakly affected,
but for other profiles this is no longer always the case. In prac-
tice, surfaces may anneal, and this may or may not mean that
the surface measured is no longer representative of the original
surface. However, the annealing of the surface does improve
the quality of the measurement. Analytical relationships are
provided for the mean height, the roughness and the fraction of
the surface actually contacted as a function of the tip radius and
the extent of annealing. For good-quality measurements, from
equations (4) and (14), the parameters δ or Δ should be greater
than 4(Rσ)0.5 and, with dimensions in nm and with the finest
tips with R = 1 nm, δ or Δ should be greater than 4σ0.5, which
is a feasible but rarely met criterion. It should be stressed that
these conclusions are for surfaces with uncorrelated heights
from point to point. Many surfaces do show such correlations,
and for those correlations that exceed the distance 4(Rσ)0.5, the
results from this study would indicate that good-quality mea-
surements should be feasible.
Acknowledgments
The author would like to thank C A Clifford, A Yacoot and
the reviewers for helpful comments. This work forms part
of the Chemical and Biological programme of the National
Measurement System of the UK Department of Business,
11
M P Seah
Innovation and Skills, with funding by the European Union
Seventh Framework Programme project NATURAL.
© 2014 Crown copyright.
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