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Development of a novel nanoscratch technique for quantitative measurement of ice adhesion strength

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The mechanism for the way that ice adheres to surfaces is still not well understood. Currently there is no standard method to quantitatively measure how ice adheres to surfaces which makes ice surface studies difficult to compare. A novel quantitative lateral force adhesion measurement at the micro-nano scale for ice was created which shears micro-nano sized ice droplets (less than 3 μm in diameter and 100nm in height) using a nanoindenter. By using small ice droplets, the variables associated with bulk ice measurements were minimised which increased data repeatability compared to bulk testing. The technique provided post- testing surface scans to confirm that the ice had been removed and that measurements were of ice adhesion strength. Results show that the ice adhesion strength of a material is greatly affected by the nano-scale surface roughness of the material with rougher surfaces having higher ice adhesion strength.
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Development of a novel nanoscratch technique for quantitative
measurement of ice adhesion strength
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International Conference on Materials Engineering and Applications IOP Publishing
IOP Conf. Series: Materials Science and Engineering 348 (2018) 012003 doi:10.1088/1757-899X/348/1/012003
Development of a novel nanoscratch technique for
quantitative measurement of ice adhesion strength
T Loho1 and M Dickinson2
1 PhD Student, Department of Chemical and Materials Engineering, University of
Auckland, Auckland, NZ
2 Senior Lecturer, Department of Chemical and Materials Engineering, University of
Auckland, Auckland, NZ
E-mail: tloh003@aucklanduni.ac.nz
Abstract. The mechanism for the way that ice adheres to surfaces is still not well understood.
Currently there is no standard method to quantitatively measure how ice adheres to surfaces
which makes ice surface studies difficult to compare. A novel quantitative lateral force
adhesion measurement at the micro-nano scale for ice was created which shears micro-nano
sized ice droplets (less than 3 µm in diameter and 100nm in height) using a nanoindenter. By
using small ice droplets, the variables associated with bulk ice measurements were minimised
which increased data repeatability compared to bulk testing. The technique provided post-
testing surface scans to confirm that the ice had been removed and that measurements were of
ice adhesion strength. Results show that the ice adhesion strength of a material is greatly
affected by the nano-scale surface roughness of the material with rougher surfaces having
higher ice adhesion strength.
1. Introduction
Ice formation and adhesion can lead to various hazards and economical losses in modern society. For
example, the presence of ice under aircraft wings or boat hulls increase the vehicles weight and drag
coefficient [1], impairing their performance. In areas with extreme winters, accretion of ice can lead to
downed power lines and road blocks [2]. One solution to this problem is to remove the ice using
mechanical or thermal methods (active de-icing), but this is energy intensive [3]. Recent literature has
instead focussed on passive de-icing methods which create a surface that prevents ice from building up
on the surface. This can be done by minimising the formation of condensation of water on the surface
or improving the roll-off behaviour of the condensed droplets which prevent frost formation [4-6].
Other researchers have tried to prevent ice formation by reducing the mechanical adhesion shear stress
of the ice-substrate interface. This includes various coatings [6,7], textured surfaces [8], or infusing
porous surfaces with liquid lubricants [9].
The effectiveness of these methods is usually characterised by measuring the ice adhesion strength,
defined as the shear stress required to remove ice from the surface. Various methods were developed
to measure ice adhesion strength at the macro-scale, for example by mechanically shearing solid ice
structures [10], using torsion to shear ice layer from a pillar [11], or using centrifugal force [12]. These
methods produce different results from one another for the same surface because there are numerous
variables that affect the results such as the shape and size of ice, loading rate, time of contact, sample
cooling rate, sample size, and many more [11]. Table 1 shows the values of ice adhesion strength of
polished stainless steel measured with different testing methods done by various researchers.
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IOP Conf. Series: Materials Science and Engineering 348 (2018) 012003 doi:10.1088/1757-899X/348/1/012003
Table 1. Values of ice adhesion strength measured with different testing methods for stainless steel
Literature
Year
Surface Temperature (°C)
Raraty, L et al [13]
1958
-10
Jellinek, H [14]
1959
-4.5
Petrenko, V et al [15]
1999
-10
Chen, J et al [16]
2014
-15
Ling, E et al [17]
2016
-15
Matsumoto, K et al [18]
2016
-5
Micro-nano scale ice adhesion strength testing can give more objective results of ice adhesion strength
and reduce some of the variables which affect macro-scale ice adhesion strength. Matsumoto et al
demonstrated this by measuring the true ice adhesion strength of various materials in the nano-scale
using Scanning Probe Microscopy (SPM) technique and found that the ice adhesion strength of a
surface is higher than what was previously measured in the macro-scale [18-20].
In this study, a new way to measure ice adhesion strength using a nanoscratch technique was
investigated. This is based on a technique developed by Dickinson et al to measure true adhesion
strength of microscopic ceramic cold-spray splats [21]. By controlling the temperature of the sample
during nanoindentation test, micro-nano sized water droplets can be condensed on the surface that will
then freeze into micro-nano sized ice droplets. Using nano-scratch technique as the basis, the ice
droplets can be sheared off the surface and ice adhesion strength can be measured.
Stainless steel was selected as a sample due to its common use in commercial and engineering
applications [22]. Xenon was used as the inert gas ion source due to its high atomic mass (131.29
g.mol−1) which leads to a higher sputtering yield than lighter noble gases. Studies have shown that
nano-scale ripple patterns arise during ion implantation and the formation is dependent on the angle of
incidence of the ion beam as well as the crystallographic orientation of the grains [23, 24]. In metals,
the ripples have been found to vary between different grains on the surface, which has been attributed
to preferential sputtering of metal grains with different crystallographic orientations on the surface
[25], impurities, and surface atom diffusion [26, 27].
2. Experimental procedure
2.1. Stainless steel samples
Grade 316 stainless steel with a BA (Bright Annealed) surface finish was cut into six 10 × 12 mm
pieces and then cleaned with acetone wipes. The samples were 1 mm thick. The BA surface finish is
the industry standard for a smooth, bright, reflective stainless steel surface according to the Standard
Specification for General Requirements for Flat-Rolled Stainless and Heat-Resisting Steel Plate, Sheet,
and Strip ASTM A480/A480M standard.
Five of the samples were ion implanted with Xe+ ions to induce atomic sputtering and create sub-
micron features on the surface of the stainless steel. Xe+ ions were extracted from a Penning ion
source at an accelerating voltage of 20 kV and selected with a 90° mass analyser magnet [28]. To limit
a significant increase in the temperature of the samples, the ion beam current density for all ion
implantation experiment was kept within 7 to 10 µA.cm2. These ions were then implanted into the
surface with different fluences ranging from 1016 to 1018 ions.cm2 at and 45° angle of incidence to
promote nano-scale features formation. During ion implantation, the pressure of the chamber was at 7
× 105 Pa. Table 2 shows the different ion implantation conditions applied to the sample. Simulation of
the ion implantation using the Dynamic Transport of Ion in Matter (D-TRIM) software [29] yielded
sputtering depths shown in Table 2.
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IOP Conf. Series: Materials Science and Engineering 348 (2018) 012003 doi:10.1088/1757-899X/348/1/012003
Table 2. Different ion beam treatment conditions on the stainless steel substrate. The sputtered depths
were calculated using the D-TRIM software.
#
Sample Name
Fluence (ions.cm-2)
Incident Angle of Ions
Sputtered Depth (nm)
1
Control
n/a
n/a
n/a
2
1E16Xe0
1 × 1016
8.56
3
5E16Xe0
5 × 1016
39.3
4
1E17Xe0
1 × 1017
86.8
5
1E17Xe45
1 × 1017
45°
162
6
1E18Xe45
1 × 1018
45°
1670
2.2. Topography measurement
The samples were cleaned using an ultrasonic acetone bath for 5 minutes prior to characterisation. The
surface roughness of the samples was characterised using a Bruker Contour GT-K Optical Profiler to
measure Root Mean Square (RMS) roughness (Rq) values. With a 5× objective magnification lens and
operating under the VSI mode, the optical profiler provided a vertical resolution of 3 nm and a lateral
resolution of 2 µm. Vision64 software (Bruker) was used to analyse the data and generate 3D profile
images. Five 960 × 720 µm rectangular measurements at random spots on the surface of each sample
were taken and averaged. SEM images were captured using an FEI Quanta 200F Scanning Electron
Microscope. Secondary electrons were detected by an Everhart-Thornley Detector.
2.3. Micro-nano scale ice adhesion strength testing
Nanoscratch testing was carried out using the Hysitron TI-950 Triboindenter machine with a 3 µm
fluid cell diamond cono-spherical tip (Hysitron). A fluid cell tip was used because of its extended shaft
made from a ceramic-based material (Macor) that prevents thermal conduction from the piezoelectric
transducer of the nanoindenter that could melt the ice droplets during testing. Humidity of the testing
chamber was controlled by flowing dry N2 gas into the testing chamber until the relative humidity was
measured to be 15%.
Surface temperature was controlled using a custom-made thermoelectric cooling device with a mild
steel base plate on the cold side and a water-cooled heat sink on the hot side. The schematic of this
device is shown in Figure 1. The cooling stage is based on a 195 W thermoelectric Peltier cooler
module (APH-199-17-10-E, European Thermodynamics). An aluminium heat sink with a heat transfer
area of 2.6 × 103 m2 was constructed to remove heat from the hot side of the module. The heat sink is
connected to a peristaltic pump that circulates 3 mL.s1 of cold water (approximately 15°C) inside it.
The plastic casing and screws were 3D-printed ABS polymer designed to prevent heat loss to the
surrounding environment and compress all the components together, removing any air bubbles
between them.
Temperature reading is obtained from a thermistor (MP-3193, TE Technology Inc.) that reads the
temperature of the mild steel base plate. To control the temperature, the Peltier module and the
thermistor is connected to a Pulse Width Modulation (PWM) temperature controller (TC-48-20, TE
Technology Inc.) that controls the voltage applied to the module based on the temperature reading
from the thermistor. To promote thermal conduction between the heat sink, the Peltier module, the
thermistor and the mild steel base plate; a layer of high-density polysynthetic silver thermal compound
(Arctic Silver 5, Arctic) was applied between them. The whole stage was then placed in a safety wall
made from mild steel to prevent spilling of water to the nanoindenter stage in case of leakage. The
sample was fixed on the mild steel base plate using a small amount of cyanoacrylate adhesive.
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Figure 1. Custom made
thermoelectric cooling
device for sub-zero tem-
perature nanoscratch
testing. (a) Assembled
view. (b) Exploded view
of the components: (1)
Plastic screws (2) Insu-
lating plastic casing (3)
Mild steel base plate (4)
Thermistor (5) 195 W
Thermoelectric Peltier
module (6) Water
cooled aluminium heat
sink (7) Safety walls to
prevent spilling of water
in case of leakage.
The micro-nano scale ice adhesion strength testing started with performing indents on the surface to
serve as a landmark, and then performing a Scanning Probe Microscopy (SPM) scan on the area by
rastering a 20 × 20 µm surface of the sample at room temperature with the nanoindenter tip set at a 2
µN force setpoint. From this point onward, this image is referred to as the ’Pre-Test’ SPM scan.
After the pre-test SPM scan was obtained, the nanoindenter tip was raised 100 nm above the surface
and the cooling stage was turned on to reduce the surface temperature to −5◦C. This process took
approximately 2 minutes before the temperature was stable, as shown in Figure 2. During this time,
water droplets condensed from the surrounding air and subsequently froze into ice droplets. Due to the
high thermal conductivity of the diamond tip, this process also significantly cooled the diamond cono-
spherical tip of the nanoindenter and prevent melting of the ice droplets during nanoscratch testing.
Figure 2. Temperature of the
mild steel base plate over time as
the cooling stage is turned on.
During testing, the temperature
remained stable at −5 ± 0.5°C for
at least two continuous hours.
After more than two minutes had passed and the surface temperature had stabilised at −5°C, the tip
was lowered into contact with the sample. Another 20 × 20 µm SPM scan of the surface was done
with the nanoindenter tip set at 2 µN force setpoint at −5°C. This image is called the ’Pre-Scratch’
SPM scan image. New features that were found in the Pre-Scratch image that were not in the Pre-Test
image were assumed to be ice droplets that formed on the surface of the sample. A sample comparison
between the Pre-Test and Pre-Scratch image of the polished stainless steel substrate is shown in Figure
3. The diameter of the ice droplet was measured using the Hysitron TriboView software to analyse the
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IOP Conf. Series: Materials Science and Engineering 348 (2018) 012003 doi:10.1088/1757-899X/348/1/012003
Pre-Scratch image. Testing was done on ice droplets that are smaller than 3 µm in diameter (less than
the tip’s radius of curvature) to ensure the nanoscratch tip sheared the whole ice droplet and not cut
through it. Once a suitable ice droplet had been found, the tip was centred above that particular ice
droplet.
Figure 3. Gradient Forward (GF) images of the (a) Pre-Test SPM scan at room temperature and (b)
Pre-Scratch SPM scan at −5°C of the polished stainless steel sample. Note that the blurriness of the
Pre-Scratch image at (b) is due to the slight vibration caused by cooling water running in the heat
sink. The circle on the Pre-Scratch image indicates the ice droplet that formed during the test. The
tip had sliding effects at lines where the ice was found due to the slipperiness of ice droplets.
The nanoscratch test began with the tip moving 5 µm vertically to measure the tilt of the sample. The
testing procedure consists of three steps, shown in the load function in Figure 4.
1. Pre-Scan scans the surface of the sample as the nanoindenter tip is moved 10 µm vertically
with 0 µN axial force. The purpose of this step is to ensure that the ice droplet to be scratched
is on the path of the nanoscratch test.
2. Scratch moved the tip 10 µm vertically in the other direction with 150 µN axial force to apply
shear stress and remove the ice from the surface. 150 µN is selected as the axial force through
trial and error as the amount of force large enough to remove the ice from the surface but not
large enough to make the tip dig through the steel surface.
3. Post-Scan scans the surface of the sample 10 µm vertically after the nanoscratch was done to
confirm removal of the ice droplet.
Figure 4. The load function of the nanoscratch testing procedure. The top graph shows the normal
force actuated on the tip over time, while the bottom graph shows the lateral displacement of the tip
over time. The load function was divided into three steps during the ice adhesion strength
measurement.
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3. Results and discussion
3.1. Sample topography
Optical profilometry revealed that for the first four fluences, the ion implantation process slightly
increases the surface roughness of the steel. The ion implantation process creates roughness features
on the surface of the steel through atomic sputtering from the xenon ions. On the 1E18Xe45 sample, it
can be seen that the roughness increased significantly and a much rougher surface was created. The
RMS roughness values and the 3D surface plot of the samples are shown in Figure 5.
Figure 5. (a) RMS roughness and (b) 3D surface plot of the polished and ion implanted stainless
steels with different fluences obtained from the optical profiler. Error bars show one standard
deviation from five repeat measurements.
In order to confirm the presence of sub-micron scale features on the surface of the stainless steel, SEM
images were taken at random spots on the surface of the samples, shown in Figure 6. Other than the
1E18Xe45 sample, the surfaces were seen to be relatively smooth with shallow roughness features. In
the 1E18Xe45 sample, it can be seen that there are ripple patterns within the grain of the ion implanted
samples, contributing to the increased roughness values measured by the optical profiler.
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Figure 6. Secondary electrons SEM images of the (a) Control sample, (b) 1E16Xe0 sample, (c)
5E16Xe0 sample, (d) 1E17Xe0 sample, (e)1E17Xe45 sample, and (f) 1E18Xe45 sample.
3.2. Nanoscratch result analysis
To prevent overestimation of the ice droplet’s diameter from the SPM scan due to the slipperiness of
ice, the vertical distance of an ice droplet is measured from the Pre-Scratch SPM scan image with the
Hysitron TriboView software. This is shown for the polished steel in Figure 7a and 7b and the effect is
illustrated in Figure 7c. As can be seen from Figure 7b, if the horizontal distance was taken, the
diameter of the ice can be overestimated by more than double the actual diameter of the ice. In this
example, the ice droplet scratched was 0.74 µm in diameter and 74 nm in height. Since the ice droplet
was relatively small, it can be assumed that the condensed droplet had a circular area of contact with
the surface.
Figure 7. Determination process of an ice droplet diameter. (a) Pre-Scratch SPM image of an ice
droplet; (b) Line topography profile of the SPM image shown in (a); and (c) Schematic showing
why vertical distance was taken as the diameter of the ice droplet instead of the horizontal distance.
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Once the size of the ice droplet was determined, a nanoscratch test according to the load function
shown in Figure 4 was performed. A sample scratch result for the ice droplet measured in Figure 7a is
shown in Figure 8. The analysis started by looking at the top right graph of normal displacement over
time during the Pre-Scan step (t = 5 to 21 s). The presence of ice was confirmed by the bump
(approximately 75 nm in height, similar to the ice droplet measured in Figure 7a) detected by the tip.
The next step was to find the position of this bump during the Scratch step of the load function. This
was done by drawing a horizontal line from the position of the ice droplet at the bottom right graph of
lateral displacement over time. At this position, it can be seen in the bottom left graph of lateral force
over time that the tip measured a jump in force when the ice was scratched. In this example, the lateral
force was measured to be 11.1 µN and this value was taken as the ice adhesion force of the sample.
Figure 8. Scratch data obtained from the Hysitron TriboScan software during ice adhesion strength
measurement after tilt correction. The four graphs shown are (top left) normal force over time (top
right) normal displacement over time (bottom left) lateral force over time and (bottom right) lateral
displacement over time.
The last step was to interpolate the position of the scratched ice to the Post-Scan step of the load
function to confirm full removal of the ice droplet from the surface, affirming that full adhesive failure
had occurred. Not all of the tests resulted in full adhesive removal of the ice droplet and sometimes the
Post-Scan step revealed that there was ice left behind after the scratch. These results were not
considered in this study as the failure involved both adhesion and cohesion.
The ice adhesion strength of the sample was then calculated by dividing the ice adhesion force with
the area of the ice droplet measured previously. In this particular example the ice adhesion strength of
the polished steel was calculated to be 4.3 MPa, which is in the same order of magnitude as the nano-
scale ice adhesion strength of stainless steel measured by Matsumoto et al [18].
3.3. Ice adhesion strength of stainless steel samples
The experiment was repeated on ten different areas of the steel samples and the results shown in
Figure 9. It can be seen that the ice adhesion strength of the first five samples were not significantly
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IOP Conf. Series: Materials Science and Engineering 348 (2018) 012003 doi:10.1088/1757-899X/348/1/012003
different at all. This is likely because the first five samples had very similar roughness measurement
and similar surface topography.
Figure 9. Mean ice adhesion
strength of the polished and ion
implanted stainless steels from
ten repeat measurements. Error
bars show one standard
deviation.
Comparing this result with the ice adhesion strength values measured by different researchers in Table
1, it can be seen that this novel method yielded results in the same order of magnitude as the works of
Matsumoto et al [18] for ice adhesion strength measurement in the nano-scale. As previously
mentioned in Section 1, the true ice adhesion strength measured in the micro-nano scale was reported
to be higher than the ice adhesion strength measured in the macro scale. This is thought to be caused
by the absence of variables within the ice itself (e.g. impurities and air bubbles within the ice) when
the size of the ice is very small. Since those variables promoted cohesive failure within the ice and
could also induce pre-existing cracks, the ice adhesion strength measured in the micro-nano scale is
much more dependent on the properties of the surface, such as its surface energy and topography,
rather than the properties of the ice. The measured values are hence closer to the true ice adhesion
strength of the surface.
It can be seen that the ice adhesion strength of the much rougher 1E18Xe45 ion implanted steel was
significantly higher than the ice adhesion strength of the smoother polished steel sample and the other
ion implanted samples where the roughness was not significantly modified. This is likely caused by
the fact that a rougher surface had a much higher true contact area than a smooth surface for the same
apparent contact area. This effect is illustrated in Figure 10. This is especially true in the case of ice
because as the water droplet freezes, it expanded into the asperities, removing any air bubbles that
might have been trapped between the surface of the water droplet and the solid. Because of the much
higher true contact area, there was increased interaction between the solid surface and the ice droplet.
Figure 10. Schematic showing how a
rough surface would have more true
contact area than a smooth surface for the
same apparent contact area.
4. Conclusions
A novel way to measure ice adhesion strength of materials in the micro-nano scale was developed in
this study to enable a more objective and repeatable data unaffected by various factors that influence
macro-scale ice adhesion failures. Moreover, by performing a post-scan of the surface after the
nanoscratch procedure, the complete removal of the ice could be confirmed to ensure failure through
adhesion and not cohesion which can occur in macro-scale ice adhesion tests. By performing the test
on surfaces with different roughness values, it can be seen that the true ice adhesion strength is much
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IOP Conf. Series: Materials Science and Engineering 348 (2018) 012003 doi:10.1088/1757-899X/348/1/012003
higher for a rougher surface than a smoother surface, as a rougher surface would have much higher
true contact area for the same apparent contact area.
With the development of this micro-nano scale ice adhesion strength testing method, objective
comparison between ice adhesion strength reduction studies can be made easier. The advantages of
this technique include the microscopic size of ice droplets, the force resolution of the nanoscratch
technique that can measure µN forces, the ability to do post-scans of the surface to confirm full
removal of the ice, and the stability of the substrate temperature achieved by the water-cooled
thermoelectric cooler. All of this leads to a more objective result of ice adhesion strength measurement
that are easy and repeatable.
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Acknowledgements
This work is funded by the University of Auckland Doctoral Scholarship programme with the help of
Dr. Jerome Leveneur and Dr. John Kennedy from National Isotope Centre, Lower Hutt, New Zealand.
... For example, Matsumoto et al. used scanning probe microscopy (SPM) to test the ice adhesion strength of materials at the nano-scale level and found that ice adhesion values were higher values at the nanoscale level compared to macro-scale test results [63,64]. Building upon this, in 2018, Loho et al. used a novel nanoscratch technique to determine the ice adhesion strength of materials at the micro and nano level [65]. The researchers used a fluid cell tip made from Macor, a type of ceramic, to avoid thermal conduction and prevent the melting of the ice droplets during testing. ...
... The researchers used a fluid cell tip made from Macor, a type of ceramic, to avoid thermal conduction and prevent the melting of the ice droplets during testing. The nanoscratch test consisted of three steps, where the fluid cell tip was moved up and over the sample, at certain increments [65]. During the nanoscratch, the tip was positioned 5 µm above the surface to measure sample tilt. ...
... A 2 mm diameter force probe, coated with a 1 mm layer of silicone rubber, is then placed 2 mm above the substrate, in direct contact with the ice. As mentioned by Loho et al., force probes that are metal may inadvertently interact with the ice, either by superficial surface melting if the outside environmental temperature is too high, or adhering to the ice, if the temperature is too low [65]. Therefore, by thinly coating the probe with a polymer coating, this effect may be minimized or prevented. ...
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... This study investigated the potential application of ion implantation technique to create an icephobic surface with low ice adhesion strength. The characterisation method for ice adhesion strength measurements were developed in the micro-nano scale and has been described elsewhere [11] in order to study the effect of nano-scale surface topography and chemistry modifications. Ion implantation on stainless steel using Xe + ions was used to modify surface topography and CF + ions to modify the surface chemistry. ...
... The micro-nano scale ice adhesion strength of the samples was measured using the novel nanoscratch technique described elsewhere [11]. Tests were done at −10°C surface temperature in air with an ambient humidity of approximately 35% and an ambient temperature of about 23°C. ...
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... where P is the adhesion strength, F ad is the adhesion of the sheet, S is the adhesion area of the sheet, Fmax is the maximum lateral force, and Fave is the average lateral force. Similarly, as reported by Loho et al. [53], a similar method was used to measure the adhesion strength of ice. During their study, pre-scan was first used to determine the location of the ice droplets. ...
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