International Archives of the Photogrammetry, Remote Sensing and Spatial Information Sciences, Vol XXXV, Part B5. Istanbul 2004
methods. Additionally, the pyramidal structure can be tilted
in the SEM for calibration purposes with still all of
nanomarkers visible to the electron beam. Also, due to the
slope steps of the calibration object, AFM measurements are
possible and provide the spatial information of the reference
points that is needed for the calibration of scanning electron
microscopes.
4. MEASUREMENT RESULTS
4.1 AFM measurement results
High precision AFM measurements in non-contact mode
were done at the PTB (Physikalisch-Technische
Bundesanstalt, Braunschweig, Germany). The instrument
used was a modificated SIS-AFM Nanostation III (SIS,
Herzogenrath, Germany) with strain gauges in z-direction
and lateral capacitive sensors to guarantee lateral high-
precision measurements. Although the device is not
approved for metrological measurements, results within 1%
of uncertainty in z-direction can be expected.
Alternatively, the nanomarker coordinates were measured
with a “normal”, commercially available Veeco Explorer
2000 (Veeco, Woodburry, USA) AFM in contact mode.
Nanomarker coordinates of all measurements were detected
using a geometric search routine, sensitive to sudden
changes in altitude on smooth topographies. Then, the high
precision SIS-AFM data were compared with the raw and
corrected data of the Explorer AFM (Table 2 and Figure 5).
Determination of the coordinates of the nanomarkers
depends on the accuracy of the sensor as well as on the
accuracy of the analysis used. From the analysis, a lateral
mean point error of 0.9 Pixel has been evaluated,
corresponding to a relative error of 0.0009 in a 1000 pixel
scan. The relative vertical error is about 0.002. Therefore, the
sensor is the limiting factor. This can be clearly seen, when
comparing the accuracy of the high-precision SIS-AFM with
a commercially available AFM, e.g. the Veeco Explorer we
used in our first approaches for reference point
determination. Further improvements will be possible by
measuring with an interferometrically controlled,
metrological AFM (MAFM).
|
i AFM Sa = relative Sensor ! rel. S, + Nanomarker
| Sensor | Accuracy | determination error |
I Is IT |
se TS jE
| Veeco 0.013
| calibrated | — ]-
Table 2. The accuracy of the AFM measurements and
nanomarker detection.
5. CALIBRATION RESULTS
With the nanomarker coordinates determined by high-
precision AFM, we were able to calibrate a high-resolution
field-emission SEM, the XL30 FEG as well as a XL30 ESEM
under “wet mode” (1 Torr water vapour pressure) conditions.
Calibration of the XL30 FEG was performed with 10 images
tilted by steps of 5 degrees. Calibration of the XL30 ESEM
was done with 5 images and arbitrary tilt steps. Tables 3 and
4 show the calibrated magnification factor (m), the mean
lateral (mxo, myo) and the mean tilt angle error calculated
(mq, mk, mo).
5.1 SEM calibration results
ETT NEUE EET NIE
| scale (m) [0.094 [pixel/nm]
| mean (mxo, Myo) [nm] | 13.03, 13.15 [nm] —— |
| mean (me, mx, me) | 0.781, 0.804, 0.248 [deg] |
Table 3. Calibration results of the XL30 FEG scanning
electron microscope.
5.2 ESEM calibration results
[Sensor
scale (me
| mean (mxo, Myo) . |l!
| mean (mg, mx, mow) | 0.
[0.1133 [pixelnm] —
| 10.228, 10.075[nm]
6
—
43, 0.654, 0.18 [deg] UT
i
Á i
e
Table 4. Calibration results of the XL30 ESEM scanning
electron microscope.
5.3 Spatial intersection and triangulation
Results of the XL30 FEG calibration were tested by applying
spatial intersection or triangulation formulas to the
nanomarker image coordinates.
Section y-z (Nanomarkers 13 - 18)
NS ee ere re YY =
| | * Spatial Intersection -
calibrated values
4- Triangulation - calibrated
values
20005600 1 re — © © Triangulation - REM settings
-T VV
T + © SIS-AFM
| ^ | A
1500.0000 + ed e i A Veeco AFM
T |
& i ; |
| m
1000.0000 + - + } MM iE
| A | =
500.0000 +
i o2 | i | i sd
NOS
-5500.0000 -4500.0000 -3500.0000 ~260C.0000 -1500 0000 -500.0000 500.0006
x [nm]
Figure 5. Section in y-z of nanomarkers 13-18 from AFM
measurements and from applying spatial intersection or
triangulation formulas.
The nanomarker coordinates in Figure 5 were calculated
either from the calibrated values or from the microscope and
tilting stage settings. Spatial nanomarker data from SIS-
AFM and Veeco AFM are shown for comparison. In lateral
direction, we found a good match of the calculated
coordinates of the REM data with the AFM measurement.
However, in vertical direction errors up to 5% did occur.
Comparison of SIS-AFM and Explorer AFM data showed
great discrepancy, even with calibrated Explorer data.
Therefore, the importance of using high-precision AFM for
accurate 3D micro-measurements is clearly underlined.
5.4 Correlative investigations
The calibration object has been tested preliminarily for other
3D micro-measurement methods, e.g. CLSM (Leica,
Bensheim, Germany) and laser profilometry (Nanofokus,
Oberhausen, Germany). Resolution of both measurement
methods is insufficient to visualize the nanomarkers, but
profile plots of the CLSM and profilometer measurements
were compared to the original high-precision AFM
measurement (Figure 6).
z [nm]
Fi
Sii
th