Measurement: Sensors 18 (2021) 100109

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Measurement: Sensors
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Metrological atomic force microscope for calibrating nano-scale step height standards

A R T I C L E I N F O A B S T R A C T

Keywords
He-Ne laser Displacement interferometer
Atomic force microscope (AFM)
Nano-scale step height standards
Measurement uncertainty analysis
In this paper, we described a metrological AFM in order to calibrate step height standards used as transfer ar­
tefacts for commercial AFMs. With X, Y and Z axes laser displacement interferometers installed, related cali­
brated results are directly traceable to the SI of metre definition. The step height measurement accuracy was
verified using several step heights up to 2000 nm. Corresponding measurement uncertainty in step height
standard calibration was estimated in line with the Guide to the Expression of Uncertainty in Measurement
(GUM). The expanded measurement uncertainty (k = 2) was better than 2.5 nm over a full range of up to 2000
nm. This suggests that the developed metrology system is capable of conducting nano-scale metrological stan­
dard calibration which is applicable to disseminating accuracy and traceability to commercial AFMs and optical
microscopes in application of surface topography measurement.

1. Introduction
Atomic Force Microscopy (AFM) [1] has already become a popular
measurement means to characterize the properties of surfaces down to
the nanometre scale and hence are adopted to be of importance tool in
the building up nanometrology infrastructure. There are a number of
standard artefacts available to do calibration of AFM scanning image
scales. In order to properly calibrate X-axis and Y-axis scales in AFMs,
either lateral 1-dimensinal or 2-dimensional regular structures are
usually employed. To conduct calibration of the Z axis scale, a series of
known step heights are usually being used. To do accurate calibration on
those artefacts, a metrological-AFM with laser interferometers installed
is necessary to provide corresponding reference values on those step
height standards in the area of nanometrology so as to enable the
measurement to have a direct measurement traceability to SI unit of the
metre, which is defined as the length of path travelled by light in vacuum
during a time interval of 1/299 792 458 of a second.
AFMs for nanometrology have been researched widely by national
metrology institutes to build up metrology infrastructure to enable ac­
curate step height standards capabilities [2–6]. National Metrology
Centre (NMC), A*STAR, Singapore, has also developed a
metrological-AFM [7] primarily to conduct measurement and calibra­
tion of those step height standards to transfer accurate traceable cali­
bration to other normal AFMs. In this paper, the system’s configuration
and calibration implementation on nanoscale step height artefacts are
briefly presented. Besides, measurement uncertainty is evaluated for
demonstrating an assurance in nano-scale step height calibration.
2. Description of the metrological AFM
Commercially available AFMs have been widely employed to capture
surface topography with a nano-scale resolution for a number of
different surface structures. Corresponding X, Y and Z surface
topography scales are typically calculated by the voltages applied on the
piezo-electric transducer (PZT) stage or PZT tube to result in a relative
linear scanning motion of a sharp AFM tip and the test sample surface.
Basically, the feedback sensors, e.g., capacitive sensor, linear voltage
differential transducers (LVDT), strain gauge and optical sensors, are
used in the close-loop control for determining those scales as well as
accuracy of the stage movement in the order of hundred micrometers for
stage and tens of micrometers for the tube. The calibration of those
scales of PZT could be implemented by the use of pre-calibrated refer­
ence standard samples/artefacts. However, due to the inherent natures
of PZT, such as nonlinearity, hysteresis, drifting, creep and aging effects,
the resulting image is always distorted. Obviously, from metrological
point of view, it is noted that there is no good enough accuracy obtained
by only doing calibration of the scales of the PZT with feedback sensors,
especially in a large scanning range up to millimetres. Therefore, it is
necessary to take laser interferometer as a displacement sensor to be
integrated into each scanning axis of the motion stage to provide a direct
traceability of the measurement/calibration in line with the national
standard of length ─ definition of the metre.
2.1. Description of AFM probe and 3D nano-scale moving platform
An AFM tiny tip in a nominal radius is less than 10 nm attached onto
a cantilever. It is sensitive to nano-scale surface topography variation, as
shown in Fig. 1, AFM head [8] has an AFM cantilever with a tiny tip
driven by an Z piezo crystal, a Piezo linear motor introducing a
displacement in a direction of Z aixs and those Clamp piezos mounted at
separated positions inside he housing Tube. A larger approaching
movement either up or down moving along the z-axis is performed to
keep the cantilever in the same bending status. In this case, the AFM
head with its AFM tip cantilever keeping in a constant bending status is
used as a zero indicator to trace the testing surface dynamically during
the AFM tip scanning over the surface. Referring to an inchworm

https://doi.org/10.1016/j.measen.2021.100109

Available online 20 September 2021

S. Wang
Fig. 1. Description of the inchworm moving for AFM head approaching the
testing surface.
Fig. 2. A schematic of a nano-scale platform.
principle, the scanning Piezo linear motor is capable of adjusting AFM
cantilever in AFM head gently and smoothly approaching the testing
surface with a stepwise up and down scanning with a moving step-wise
size less than 0.5 μm. A total Z movement range is up to 5 μm during
AFM head scanning along Z-axis to collect surface topography infor­
mation in the measurement.
Fig. 2 shows a schematic diagram of a nano-scale platform produced
by SIOS Messtechmik GmbH [9]. The platform has a linear positioning
range of 25 mm × 25 mm × 5 mm along X, Y and Z axes respectively.
The platform is able to provide a minimum moving step in an order of
0.1 nm and a moving linear displacement with an accuracy in order of
several nanometres. The AFM probe in use can be mounted above the
stage using the three (3) cylindrical holders made from Zerodur to
ensure its thermal stability. Since the Zerodur material has a very low
thermal expansion coefficient (α is about 0.02 × 10− 6/◦ C), the three
holder can stably keep all relevant measurement components, including
AFM head, laser interferometers and mechanical parts, with minimum
drifts during the measurement in the system. There are 3 He–Ne laser
linear displacement interferometers for directly determining each axis’s
linear displacement. Meanwhile, another two infrared optical auto­
collimation angular sensors are used to synchronously correct
nano-scale stage angular movement errors, such as the corner mirror
block’s yaw, pitch and roll angle deviation during AFM scanning with
respect to the testing surface. Therefore, the stage can always move in
parallel along X, Y and Z axes accordingly. In addition, it is worthy of
noting that the cantilever tip in AFM head is pre-adjusted to put it to be
at the virtual interaction point of the three laser interferometers in order
to make the AFM scanning direction in line with the Abbe principle. In
this case, there is a minimized Abbe offset error in the proposed
2
Measurement: Sensors 18 (2021) 100109
Fig. 3. The system in operation.
metrological-AFM system.
2.2. Arrangement of the proposed system
A photograph of the metrological-atomic force microscope (M-AFM)
built in our centre is shown in Fig. 3. It is noted that system is located
inside a clean booth (class 100) environment to mainly provide a clean
environment to minimize possible dust containment onto he testing
sample. Also, there are an isolation table and an acoustical enclosure
taken into account keeping the system prevented from external me­
chanical vibration & sound effects in order to ensure the system working
environmental condition with less impacts to a high accurate measure­
ment and calibration.
3. Uncertainty analysis
In terms of the ISO guide to the expression of the uncertainty in
measurement (GUM) [10], the step height expanded measurement un­
certainty in the proposed system can be evaluated through considering
possible known source of errors. The step height (h) may be defined as
follows:
( )
h= N
c cos θt
+ LAbbe + Ldp + Lmf *[1 − α(T − 20)] (1)
2nf0 cos θm
Where.
N is the separation in interference fringes in the z axis of the two
surfaces including step’s top & bottom sections on an area of interest
on the step depth in terms of ISO 5436-1
c is the light speed in vacuum.
n is the environmental air refractive index.
f0 is the He–Ne laser frequency
θm is laser incident angle with respect to laser reflective corner
mirror surface
θt is the residual deviated angle of the actual scanning axis with
respect to and the measurement axis
LAbbe is a resulting Abbe offset error
Ldp is a resulting error from the length of dead path in laser
interferometer
Lmf is a resulting error from the thermal expansion about its metro­
logical frame
T is an averaged temperature during step height measurement
αis the sample’s thermal expansion coefficient
In terms of GUM, corresponding step height measurement uncer­
tainty budget could include contributions of type A and type B.
The type A standard uncertainty is evaluated from a measurement
repeatability to reflect the system measurement stability. Using a set of
21 step height measurements on a step height of 2000 nm, the resulting
S. Wang Measurement: Sensors 18 (2021) 100109

Table 1
Uncertainty budget for the step height calibration & measurement using LRM-AFM, number of measurements m = 21. Nominal values in use: laser frequency f0 =
474′ 1012 Hz, light speed c = 3′ 108 m/s, Vacuum air refractive index n = 1, Step height h, Abbe offset δ = 1 mm, dead path dp = 2 mm, misalignment angles qm = 6◦ and
qt = 7◦ , Averaged temperature T = 22.60 ◦ C.
i Quantity Xi Uncertainty u (xi) Probability Sensitivity coefficient Uncertainty contribution ui(h) Degrees of freedom
distribution ci (nm) vi

1 Interferometer data, N 0.0015 fringe R 316.4 (nm) 0.47 ∞

2 Vacuum frequency, f0 5.47 × 106 Hz R 2.11 × 10− 15
h (nm/ 1.15 × 10− 8h ∞
Hz)
3 Air refractive index, n 0.71 ppm N h (nm) 7.1 × 10− 7h ∞
4 Cosine error, θm 2739 ppm N 0.10h (nm) 2.74 × 10− 4h ∞
5 Cosine error, θt 3726 ppm N 0.12h (nm) 4.47 × 10− 4h ∞
6 Abbe error, LAbbe 0.56 nm N 1 0.56 ∞
7 Dead path,Ldp 0.12 nm R 1 0.12 ∞
8 Metrology frame expansion correction, 0.023 nm R 1 0.023 ∞
Lmf
− 7 − 9
9 Temperature, T 0.015 ◦ C R 5.0 × 10 h (nm/◦ C) 7.5 × 10 h ∞
10 Thermal coefficient α 1.2 × 10− 6/◦ C R 2.6h (nm.◦ C) 3.12 × 10− 6h ∞
11 Measurement repeatability, R 0.084 nm @2000 – 1 0.084 20
nm

Fig. 4. A typical result of a step height standard (a nominal value: 8 nm step

height) measured by the proposed system: 2D plot to show one of cross-section
perpendicular to step.

Fig. 5. A typical result of an undercut step height standard (a nominal step

type An uncertainty u(R) of the system is less than 0.084 nm, which height value: 1800 nm) measured by the proposed system: a 2D plot to show
mainly indicates random errors in the system. The relevant sources of one of cross-sections.
type B uncertainties in the proposed system can be given in Table 1.
As an error budget for any particular measurement may be calculated /
from appropriate summation of the estimated values of the individual 4
∑
11
( )
veff = [uc (h)] u4i (h)/vi
contributions given above. Table 1 shows those uncertainty (3)
i=1
components. /( )
In accordance with GUM, corresponding combined standard uncer­ = 1.284 0.0844 ÷ 21 = ∞
tainty attributed to h can be calculated by the root sum squared of all From the t-distribution table, for a confidence level of approximately
errors in Table 1. 95%, the expanded measurement uncertainty is given by
From the t-distribution table, for a confidence level of approximately
95%, the expanded measurement uncertainty is given by U(h) = k ·√
uc ̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅
(h)
(4)
[ ]12 =2 × 0.746 2
+ ( 0 . 52 h )2
∑
11
uc (h) = u2i (h) × h2 Therefore, the expanded measurement uncertainty of step height (h)
calibration in quadrature is as follows:
i=1

{( ) [( )2 U(h) = Q[1.5, h] nm, h in micron, estimated at a level of confidence of

= 0.472 + 0.562 + 0.122 + 0.0232 + 0.0842 + 1.15 × 10− 8
approximately 95% with a coverage factor k = 2.
( )2 ( )2 ( )2
+ 7.1 × 10− 7 + 2.74 × 10− 4 + 4.47 × 10− 4
( )2 ( )2 ] }12 4. Verification results of step height measurement
+ 7.5 × 10− 9 + 3.12 × 10− 6 × h2
√̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅ In order to verify step height measurement accuracy in the proposed
= 0.7462 + (0.52h)2 (2) system, three step height standards have been utilized. The measure­
h in micron, the effective degree of freedom for uc (h) is given by ment results are described as follows.
A protrude step height standard with a nominal value of 8 nm was
measured. As shown in Fig. 4, its 2-dimensional (2D) AFM scanned re­
sults were obtained. Based on the step height calculation method

3
S. Wang
defined in ISO 5436–1 [11], corresponding mean measured step height
was determined to be 8.6 nm with an expanded measurement uncer­
tainty of 1.5 nm. In comparison of the measured value to its reference
value (8.5 ± 1.7) nm certificated by National Physical Laboratory (NPL,
UK), there is a deviation of 0.1 nm, which demonstrated that the step
height measured is favorably comparable to the reference value.
An undercut step height standard artefact having a nominal step
height value of 1800 nm was calibrated by NPL and its reference value
was reported to be (1785.9 ± 3.8) nm. Corresponding 2D plot results
were obtained as shown in Fig. 5. The mean measured step height was
measured to be 1785.6 nm with an expanded measurement uncertainty
of 2.5 nm by the proposed system. The deviation of 0.3 nm from the
reference value is 0.3 nm. Similarly, taking into account the measure­
ment uncertainty of 3.8 nm from NPL, the measured value is also
favorably comparable to the reference value. Therefore, the proposed
system is capable of conducting a nana-scale step height measurement &
calibration.
5. Conclusions
In this paper, a metrological atomic force microscope and its step
height measurement uncertainty have been described. The developed
system is composed of an AFM for surface detection, a three-axis nano-
positioning stage for sample holding and scanning, control electronics &
software, an anti-vibration isolated platform and acoustical enclosure.
In the experiment for verifying measurement uncertainty, step height
standards have been utilized to validate its nano-scale accuracy mea­
surement performance. Both experimental results and measurement
uncertainty evaluation demonstrated that the system is able to provide a
nano-scale measurement uncertainty in step height calibration. Because
three (3) He–Ne laser linear displacement interferometers are built in
along three (3) axes (X, Y and Z) in the system, the proposed
metrological-AFM is then capable of providing a direct traceability of
step height measurement & calibration to disseminate a higher accuracy
to those commercial AFMs and high resolution 3D optical microscope for
Measurement: Sensors 18 (2021) 100109
their surface topography measurements. It covers those applications in
micro- & nano-scale structure measurements in the fields of MEMS,
semiconductor, precision engineering and photonics industrial sectors.
Acknowledgments
This research did not receive any specific grant from funding
agencies in the public, commercial, or not-for-profit sectors.
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Shihua Wang
National Metrology Centre, Agency for Science, Technology and Research
(A*STAR), 2 Fusionopolis Way, 138634, Singapore
E-mail address: wang_shihua@nmc.a-star.edu.sg.