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Calibration of Lateral Force Measurements in Atomic Force Microscopy With A Piezoresistive Force Sensor
Calibration of Lateral Force Measurements in Atomic Force Microscopy With A Piezoresistive Force Sensor
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033708-2 Xie et al. Rev. Sci. Instrum. 79, 033708 共2008兲
Author complimentary copy. Redistribution subject to AIP license or copyright, see http://rsi.aip.org/rsi/copyright.jsp
033708-3 Piezosensor AFM lateral calibration Rev. Sci. Instrum. 79, 033708 共2008兲
冑
points on the hemline of the trapezoid head on the free end of the cantilever.
The fourth curve with a lower gradient denotes the calibration result when n 12
t= , 共1兲
the contact point is on the tip of cantilever. K2n E
where Kn is the wave number on the AFM cantilever and is
gram was used to control the motion of the nanopositioning its density and n is the nth flexural resonant frequency. If
stage with a fixed increment 共20 nm in our experiment兲 n = 1, then KnL = 1.8751, where L is the length of the AFM
while the voltage output V p of the electronics was recorded. cantilever. When the dimensions of the cantilever are ob-
It was found that the displacement of the piezoresistive can- tained, the normal and lateral spring constants kn and kl can
tilever tip was approximately 5.7 m across the full range of be calculated from
the piezoresistive force sensor output. Ewt3
After 20 complete loading/unloading calibration cycles, kn = ,
4L3
we achieved a piezoresistive force sensor sensitivity
S p = 10.361⫾ 0.267 N / V. The sensitivity S p = dF / dV p is de- Gwt3
fined as the gradient of the applied force F versus the voltage kl = , 共2兲
output V p plot. 3L共h + t/2兲2
During the force calibration of the piezoresistive force where w, t, and h are the width, thickness, and tip height of
sensor, four contact points were used to test whether a posi- the AFM cantilever, respectively.
tion change on the width affects its sensitivity. As shown in Experimental methods. Once the piezoresistive force
Fig. 2, the first three contact points were located on the hem- sensor had been calibrated, it was used as a force standard to
line of the trapezoidal head on the free end, on which there determine the lateral force conversion factor ␣ of the AFM
were two points: one on each of the left and right bottom cantilevers. The experiments described below were per-
corners, and another in the center of the line. The fourth formed on a combined AFM/optical microscope system. Al-
contact point was located on the very tip of the free end. though the experiment procedure in this work may be not
Plots of the voltage output versus displacement 共applied available on all commercial AFMs, this method could be
force兲 have the same gradient except for the fourth contact widely used after some adjustment.
point, which has a lower gradient because of a lower stiff- For its actual use, the piezoresistive cantilever was fixed
ness on the tip. This experimental result demonstrated that into a metal harness with four contact clips. The cantilever
the Wheatstone resistance bridge is not sensitive to the tor- and the harness were integrated onto a thin circuit board,
sion loading applied on the piezoresistive cantilever’s longi- which was attached to the AFM stage using a fixture. The
tudinal axis. Thus, the points on the side edges as well as the electronics, including amplifier, signal filter, and power sup-
TABLE I. Descriptions of the cantilevers based on the beam mechanics and the experimental results. The cantilever’s length L, the width w, and the tip height
h were measured using the optical microscope. The first flexure resonant frequencies f 0 were used to determine the thickness of the AFM cantilevers from Eq.
共1兲. The normal spring constant kn and lateral spring constant kl were calculated from Eq. 共2兲. ␣0 calculated based on the beam mechanics from Eq. 共11兲, ␣
measured from the proposed top loading and side loading methods are listed in the last three columns respectively.
Tip No. L共m兲 h共m兲 w共m兲 t共m兲 f 0共kHz兲 kn共N / m兲 kl共N / m兲 ␣0共N / V兲 ␣共N / V兲 ␣共N / V兲
1 228 15.5 47.8 0.83 21.84 0.092 10.34 1.61⫾ 0.53 2.29⫾ 0.26 2.32⫾ 0.26
2 449 17.4 53.4 2.01 13.64 0.19 62.27 11.24⫾ 3.71 12.04⫾ 1.35 12.31⫾ 1.38
3 229 17.6 31.4 2.28 59.49 1.24 101.06 18.79⫾ 6.20 25.84⫾ 2.89 26.2⫾ 2.93
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033708-4 Xie et al. Rev. Sci. Instrum. 79, 033708 共2008兲
corner of the trapezoid head on the free end. After the load-
ing locations had been determined, the AFM tip was moved
laterally to the contact location with a step of 10 nm. Under
the programmed control, voltages V p and Vl, outputs of the
piezoresistive force sensor and the photodiode began to be
recorded at a frequency of 5 Hz when Vl reached the defined
preload value of 0.01 V. During the measurement, the de-
flection of the AFM cantilever was controlled to keep the
voltage output in the linear range of the photodiode.
Data analysis. For the top loading method, the loading
force on the AFM tip can be presented as
F t = k p␦ p = k t␦ t = S pV p , 共3兲
where kt is the total lateral stiffness of the AFM cantilever-
tip-contact system and ␦ p and ␦t are deflections of the pi-
ezoresistive cantilever and AFM cantilever tip, respectively.
Here, kt can be obtained from a sum of stiffness inverses of
each part: kt = 共1 / klateral + 1 / ktip + 1 / kcontact兲−1, where klateral is
FIG. 3. 共Color online兲 Diagrams of the experimental configurations for the the lateral stiffness of the AFM cantilever and its tip lateral
calibration of the AFM cantilevers with a piezoresistive force sensor. Two stiffness is ktip and kcontact is the contact stiffness between the
methods, termed top loading 共a兲 and side loading 共b兲, in which L p and l p are
distances from the contact points to the clamping end of the piezoresistive AFM tip and the piezoresistive cantilever surface. kcontact,
cantilever, is the mounting angle of AFM cantilever on the vertical plane which is proportional to the contact radius17 and often com-
that is through its longitudinal axis, and is the mounting angle of the parable to klateral and ktip,18 causes the lateral force calibration
piezoresistive cantilever on the horizontal plane. 共c兲 The deflections of the
to be more challenging because in this case ␦t is not equal to
piezoresistive cantilever and AFM cantilever tip are ␦ p and ␦t, respectively.
the real lateral deflection associated with the photodiode out-
put. Fortunately, in our method, the lateral conversion factor
ply, was separated in another unit. Considering the limita- is directly provided by the ratio of the applied force on the
tions of the manipulation space in the AFM, two ways were AFM tip and the photodiode’s voltage output, regardless of
recommended for mounting the piezoresistive cantilever. The any knowledge of the cantilevers and the laser measuring
first involves mounting the piezoresistive cantilever verti- system. For the top loading method, the force Ft = S pV p is
cally on the AFM stage along its longitudinal axis 关see Fig. applied on the AFM tip, so the conversion factor ␣ can be
3共a兲兴, termed top loading, which reduces the mounting area simply obtained from
at the cost of height space. In this way, the AFM cantilever
Ft Vp
tip contacts with the top edge of the piezoresistive cantilever ␣= = Sp . 共4兲
during the calibration 关see the loading location in Fig. 1共d兲兴. Vl Vl
Nevertheless, if the piezoresistive cantilever is too high For the side loading method, in order to reduce the effects of
共8 mm in our experiments兲, the piezoresistive cantilever can friction force on the contact point, the loading direction is
be mounted in the second way: horizontally on the AFM perpendicular to the piezoresistive cantilever. In this case,
stage 关see Fig. 3共b兲兴, termed side loading. Note that in this the lateral force conversion factor ␣ under the side loading is
case, shoulders of the piezoresistive cantilever substrate determined from
might be in the way of the reflected laser beam, so an angle
to the vertical plane that is through the longitudinal axis of Fs V pL p cos
␣= = Sp , 共5兲
the AFM cantilever was deliberately mounted 共 = 15° in our Vl V ll p
experiments兲. The loading location in the second method was
very close to end of the side edge 关see Fig. 1共d兲兴. where L p and l p are distances from the contact points to the
Lateral force calibration was started once the whole clamping end of the piezoresistive cantilever for top loading
setup was ready. At first, we had to find the loading locations. and side loading, respectively 共shown in Fig. 3兲.
For the top loading, after the AFM cantilever was brought However, considering that the lateral force is loaded on
into contact with the top surface of the piezoresistive canti- the side of the tip, not on the tip head of the AFM cantilever,
lever, the contact mode was used to scan the top side edge to a simple linear transformation of the factor ␣ is given by
identify its center point. Then the AFM cantilever was
moved 2 m away from the scanned side edge. In order to
ensure that the AFM tip was reliably in contact with the top
冉
␣⬘ = ␣ 1 +
⌬h
h + t/2 − ⌬h
, 冊 共6兲
side edge, the AFM cantilever was moved down with a dis- where ⌬h = 0.5– 0.8 m is the distance from the contact
placement ⌬h = 0.5– 0.8 m before being moved back to the point to the tip head of the AFM cantilever and t is the
contact location. For the side loading, the procedure was cantilever thickness. For the cantilevers used in our experi-
largely the same; the only difference being the position of the ments h = 15.5– 17.6 m and t = 0.83– 2.28 m, so an error
loading location. As shown in Fig. 1共d兲, the side loading was of the factor ␣ generated from ⌬h is 2.7%–5%, which is just
positioned at the end of the top side edge, in fact, a bottom within an acceptable range.
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033708-5 Piezosensor AFM lateral calibration Rev. Sci. Instrum. 79, 033708 共2008兲
We quantitatively compared our method with the theo- to be equal to the normal sensitivity. Thus, the lateral force
retical method based on the beam mechanics. For the conve- conversion factor ␣0 can be calculated from
nient comparison of the normal and lateral conversion fac-
Ewt3
tors, the photodiode sensitivity is defined as a ratio of the ␣0 = Sn . 共11兲
angular deflection of the AFM cantilever and the photodiode 3l共h + t/2兲
voltage for which the lateral inverse sensitivity is Sl = l / Vl, However, the hypothesis of photodiode symmetry is often
and the normal photodiode inverse sensitivity is Sn = n / Vn. not exactly the case due to the possible asymmetry of the
Here, n and l are the normal and lateral angular deflections laser spot shape as well as the diffraction effects from the
of the cantilever, respectively; Vn and Vl are the correspond- cantilever, and may induce errors.
ing photodiode voltage outputs. The beam mechanics method requires accurate knowl-
The normal spring constant kn connects the flexural de- edge of the cantilever’s elastic modulus and dimensions. As
flection xn due to an applied normal force Fn, which can be discussed below, in our experiments, the high-resolution op-
determined by35 tical microscope is used to measure the cantilever’s length,
width, and the tip height, and the force oscillation method
F n = k nx n . 共7兲
described in Eq. 共1兲 is used to determine the thickness of the
So, based on the beam mechanics, Eq. 共7兲 can be presented cantilever.
as
Fn = 32 knlSnVn , 共8兲 RESULTS AND DISCUSSION
where l is the effective length of the AFM cantilever. There- As described above, two loading methods were used in
fore, the normal inverse sensitivity Sn of the photodiode can our experiments: top loading and side loading. In the first
be determined from case, we used Eq. 共4兲 to calculate the lateral force conversion
3 dxn factor. For side loading, considering the loading position and
Sn = . 共9兲 the direction of the loading force, therefore, Eq. 共5兲 was used
2l dVn
to calculate the lateral force conversion factor. The inverse
For a cantilever with a rectangular cross section, the lateral sensitivity Sn of the photodiode described in Eqs. 共7兲–共9兲 was
force is related to the measured photodiode voltage Vl from measured for each AFM cantilever by a linear fit on the plot
Gwt3 of the photodiode voltage output versus displacement of the
Fl = S lV l , 共10兲 cantilevers. Here, we assumed that the photodiode inverse
3l共h + t/2兲 sensitivities Sl and Sn had the same value in our experiments.
where G is the cantilever shear modulus and h is the tip The experimental results are summarized in Table I,
height. Based on the laser beam mechanism, the displace- which lists the dimensions and the mechanics of the AFM
ment of the laser spot on the photodiode is decided by the cantilevers. The dimensions, including length L, width w,
reflecting cantilever’s angular deflection and the distance be- and tip height h, were measured using the optical micro-
tween the reflecting point and the spot position on the pho- scope. The first flexure resonant frequencies f 0 were used to
todiode. Normally, the distance can be considered as a con- determine the thickness of the cantilevers from Eq. 共1兲. The
stant; so, based on the hypothesis that the photodiode is normal spring constant kn and lateral spring constant kl were
“rotationally symmetric,”29 the lateral sensitivity is assumed calculated from Eq. 共2兲. The last three columns list ␣0 cal-
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033708-6 Xie et al. Rev. Sci. Instrum. 79, 033708 共2008兲
culated from Eq. 共11兲 based on the beam mechanics, and ␣ levers with normal spring constants from 0.092 to 1.24 N / m
measured using the proposed top loading and side loading 共lateral stiffness from 10.34 to 101.06 N / m兲. Compared with
methods, respectively. the calibration results of the theoretical method based on
Each cantilever was bent laterally by the piezoresistive beam mechanics, the proposed approach provides lateral
cantilever ten times. For each time the lateral force conver- conversion factor values that are accurate to ⫾12.4% or bet-
sion factor was calculated as outlined in Figs. 4共a兲–4共c兲, in ter. Moreover, this method can be used to directly calibrate
which the symbol of the blue solid circles shows data ob- the lateral force regardless of the cantilever’s geometry or
tained from the experiments using the top loading method. knowledge of the photodiode detector, thereby enabling an
The straight red lines are the linear fit of the corresponding accurate and direct calibration of the lateral force measure-
data using the least squares method; their gradients were ment of AFM.
used to calculate ␣ from Eq. 共4兲. Then, a value of the lateral
force conversion factors was averaged from the results of the ACKNOWLEDGMENTS
ten experiment repeats. The lateral force conversion factor
␣0 was calculated based on the beam mechanics. Figure 4共d兲 This work was supported by European project
shows a comparison of the lateral force conversion factors NANORAC 共Contract No. STRP 013680兲.
obtained from each method. The top loading and side loading
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