Measuring The Thickness of Thick Films With A Spectroscopic Reflectance System

Measuring the Thickness of Thick Films with a Spectroscopic Reflectance System
Measuring the Thickness of Thick Films with a
Spectroscopic Reflectance System
Sponsored by SemiconSoft Sep 20 2018
The MPROBE® can be used to precisely measure almost any translucent film with a
thickness between 1 nm and 1 mm, making it suitable in most thin film
applications.
The data from the system can be measured using two different methods, which are
model/curve fitting, or Fast Fourier Transform (FFT) analysis on the captured spectrum.
Generally, model fitting is used for thinner films (between 1 nm and 1 µm in width) and
FFT is used for films of a thickness greater than 20 µm.
Within the intermediate thickness range (1 µm to 20 µm), the use of either method is
appropriate, with the preference depending on the experimental requirements.
Figure 1. Data analysis method depending on the thickness range.
Using the Fast Fourier Transform (FFT) method can be preferential, as it has low
calibration requirements (variations in the intensity have no impact on the results), the
analysis happens quickly, and a minimal amount of prior information on the sample is
needed.
However, it is not a perfect method. FFT requires the refractive index (R.I.) information of
the materials to be known and, until recently, has provided a lower accuracy than a curve
fitting method. The accuracy of FFT has been improved by new additions to
Semiconsoft’s TFCompanion software, which now has an enhanced decomposition
algorithm. Following these improvements, the method can now deliver accuracies better
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than 0.1%.
Thickness Range of the Practical FFT Use
FFT exploits the periodicity of interference between the wavelength and intensity, a
phenomenon known as interference fringes. The material’s R.I. and the wavelength
range of the measurement determine the minimum thickness of a film, which can be
measured accurately using FFT.
This is because sampling only one period, or a fraction of a period’s function, (as would
happen for very thin films) results in poor FFT data. The measurement error of FFT
methods for different wavelength ranges and the thicknesses are given in Table 1.
Table 1. FFT measurement errors.
Thickness/ 200 500 700 1,000

Wavelength range nm nm nm nm
Error(absolute value) 92 nm 36 nm 6 nm 0.6 nm
4001,000 nm
Error (%) 46% 7% 0.9% 0.06%
Error (absolute value) 49 nm 2 nm 1.2 nm 0.4 nm
4001,700 nm
Error (%) 24% 0.4% 0.017% 0.04%
A Fast Fourier Transform method was used to analyze simulated reflectance spectra for
oxide films with widths of 200 nm, 500 nm, 700 nm and 1,000 nm, and the absolute and
relative measurement errors were calculated. Spectra were then calculated for the
measurement ranges 400 – 1,700 nm and 400 – 1,000 nm.
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Figure 1. Simulated reflectance spectrum (wavelength range: 4001,000 nm) of the
SiO2/Si. Oxide thicknesses: 200 nm, 500 nm, 700 nm and 1,000 nm (Oxide thickness
corresponding to one period in visible range is ~ 320 nm)
Figure 2. Thickness of the 200nm oxide determined using FFT (4001,000 nm
wavelength measurement range). A large thickness measurement error (92 nm) shows
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that FFT maybe not practical for this thickness
Figure 3. Thickness of the 1000 nm oxide determined using FFT (4001,000 nm
wavelength measurement range). A very small measurement error (0.6 nm) shows that
FFT can be used successfully for this thickness
Applications of FFT Analysis
Analyzing Multilayer Polymer Films
Multilayer Polymer Films have a wide application base, being used in a multitude of
‘everyday’ products, such as stickers and food packaging.
In this example, a 4layer polymer film, used as a sticker, is analyzed. The film has a
structure of separator/silicon/adhesive/PET (substrate). The silicon layer is a thin film, of
thickness less than 1 µm, which can be peeled off to leave the PET film naked. This then
behaves as an adhesive.
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Figure 4. Reflectance spectrum measured with MProbeVisHR (700 nm 1,000 nm
wavelength range). Sample 1 is a 4 layer polymer web (sticker).
Figure 5. FFT decomposition data analysis of the data (Fig. 4). Position of the peaks
indicate the thickness of the layers.
Running a Fast Fourier Transform analysis results in a peak for every interface pair,
which also correspond to layers in the multilayer film. The height of the peak can be used
to elucidate information about the interface’s quality, whereas the peak position can be
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used to determine the layer’s thickness.
As a peak is given for every interface, a threelayer stack should give an FFT spectrum
with six peaks, with the final peak relating to the total thickness of the stack. Figure 5
shows an example of this.
In Figure 5, the silicon layer (peak 3*) has too low a thickness (less than 1 µm) to be
seen individually, and instead, is combined with the separator + adhesive, and the
separator layers. The low thickness of the silicon layer means that the total thickness
peak (peak 6) is also broader.
Using TFCompanion software allows researchers to automatically determine each peak
and match them to corresponding layers. This is easier for the software if the structure of
the film being measured is known with the approximate thicknesses of each layer, which
helps each layer to be correctly identified.
If this information is not known, it can often be determined from the FFT data and then
inputted back into the model.
Figure 5 shows the FET decomposition spectrum with all of the layers shown, with the
exception of silicon. In cases where the membrane is too thin, layers can be hidden by
other peaks, or the peak can be too low to identify.
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Figure 6. Reflectance spectrum measured with MProbeVisHR (700 nm – 1,000 nm
wavelength range). Sample 2 is a 4 layer polymer web (sticker). Sample 2 has the same
structure as Sample 1 but, in this case, the thicknesses of the Separator and PET
(Substrate) layers are similar.
Figure 7. FFT decomposition data analysis of the data (Fig. 6).
Deconvolution of the FFT data from Sample 2 (as shown in Figure 7) does not show
Layer 3, however, Layer 3’s impact can be observed in the broadening of Layer 1’s peak.
Whilst the peak of L1 could be deconvoluted to give the thickness of L3, it is more
practical to use the information provided on total thickness and the thickness of L1 and
L2, to determine the thickness of L3.
Figure 8 shows how the missing thickness of a layer (e.g. L3) can be found from the total
thickness, using the software’s different thickness option.
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Figure 8. Setting differential thickness option to determine thickness of the “hidden”
layer/interface from the total thickness. Noise level setting helps separate Layer
thickness data from the noise.
Measuring an Alumina (Sapphire) Layer
Thick layers such as alumina, yttrium oxide and parylene all have a refractive index
which is highly dependent upon the layers deposition conditions. As the R.I. can be
different between samples, using data from a library or other optical properties databases
alongside the FFT method can give erroneous data.
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Figure 9. Reflectance of Alumina on glass measured with MProbe UVVisSR system
(wavelength range: 200 nm 1,000 nm)
Figure 10. FFT decomposition of the data on Fig. 8. using library Alumina material
properties. The peak position indicates the thickness of 1,164 nm
Directly comparing the library data model against measured data using an FFT method
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demonstrates that the R.I. value given in the library data is not correct.
Figure 11. Direct comparison of the FFT results model (red) and measured data (blue)
shows that R.I. is not correct.
Figure 12. Direct fit of the model to measured data to determine the thickness and R.I. of
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alumina. Thickness 1,202 nm.
Figure 13. Alumina R.I. determine from the measurement (yellow) and library alumina
R.I. (red)
Measuring Hard Coatings
Hard coatings are an essential part of many systems, such as the polycarbonate
surfaces used in automotive lighting covers and eyeglass lenses. When a hard coating is
deposited on a surface, it penetrates into the carbon, creating an Inter Penetration Layer
(IPL) which is relatively thin (approx. 1 μm).
When measuring hard coatings for QC, it is important that the thickness of both the hard
coating layer and the IPL are measured.
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Figure 14. Reflectance spectra of polycarbon with hardcoat sample (headlight).
Measurement is taken with MProbe Vis system (wavelength range: 4001,000 nm)
Figure 15. FFT decomposition of the measurement data (Fig. 14). A differential thickness
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option is activated and IPL is determined from total thickness. Hard coat: 5.2 μm, IPL:
1.85 μm
The IPL layer exhibits a refractive index which is between the R.I. values of the hard
coating and the polycarbonate layer, meaning there is a weak optical contrast between
the two different materials.
This means that the peak from the IPL is very weak. However, this issue can be avoided
by running a differential IPL thickness determination (from the total thickness) to give
more accurate results.
Improving the Accuracy of FFT Analysis
When using an FFT method, the overall accuracy of the thickness measurement is
dependent on how accurately locating the peak position. The error of this measurement
can be given using the equation: (Xn+1Xn)/2, where, as in Figure 1, Xn and Xn+1 are
points either side of the peak.
Figure 16. FFT points resolution. Distance between adjacent FFT points (bins)
determines maximum error.
Several options are available, using TFCompanion software, to improve the accuracy of
analysis, which include:
1. Interpolating between data points
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2. Fit a Gaussian function to the peak to determine the position
3. Increasing the number of data points
4. Filter the data (apodization) – indirectly improves accuracy by removing aliases and
additional peaks. Especially helpful for noisy data.
Below, these different methods are used with TFCompanion for the measurement of a
polymer film.
Figure 17. Measured reflectance spectrum of coating (~ 18 µm) on 38 µm PET
Interpolating Between Points and Applying a Gaussian
Fit
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Figure 18. Selecting accuracy level.
TFCompanion allows for three different modes of accuracy:
Maximum accuracy – A full Gaussian curve is fitted to the peak
High accuracy – Interpolation between the points using a Gaussian model
Default – No fitting or interpolation
Increasing the Number of Data Points
The data points from FFT analysis are spread over the greatest range of the thickness
measurement for which data can be gathered. However, in most cases, only a section of
this range is of interest. E.g. in this example, the sample thicknesses are only 18 µm and
38 µm whereas the thickness range of measurement is 280 µm.
The number of data points in the thickness range of interest can be increased using a
technique called oversampling.
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Figure 19. Resolution improvement by using increased number of FFT points. 1 is
default resolution, 5 – maximum resolution.
Figure 20. Peaks using default resolution (1)
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Figure 21. Peaks using high resolution (4)
Figure 22. Peak detail from fig. 20 (default resolution 1)
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Figure 23. Peak detail from Fig. 20 (high resolution 4)
Table 2. Maximum possible absolute measurement error depending on the resolution for
this measurement
Resolution 1 2 3 4
Maximum possible error (µm) 0.548 0.274 0.137 0.068
Filtering the Data (Apodization)
Figure 24. Apodization filter selection
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Figure 25. Peak without data apodization/ Two aliases are visible.
Figure 26. Peak with data apodization (peak is the same as on Fig. 25)
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Figure 27. Reflectance spectrum of GaN on sapphire (4001000 nm wavelength range)
Figure 28. Measurement of GaN (fig. 27) without data apodization
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Figure 29. Measurement of GaN (Fig. 27) with data apodization
This information has been sourced, reviewed and adapted from materials provided by
SemiconSoft.
For more information on this source, please visit SemiconSoft.
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SemiconSoft
Address
83 Pine Hill Rd
Southborough
Massachusetts, 01772
United States
Phone: +1 (617) 388 6832
Fax: +1 (508) 858 5473
Email: info@ semiconsoft. com
Visit Website
SemiconSoft, Inc is the premier source of thinfilm thickness measurement instruments.
SemiconSoft offers thin film measurement systems, optical spectroscopy tools and data
analysis software. The solutions are available for a variety of applications, from desktop
and insitu to inline measurement. From polymer thickness to optical coatings thickness,
practically any translucent material in 1 nm 1 mm thickness range can be measured
quickly and reliably :
Oxides, nitrides, semiconductors, photoresists
Thinfilm solar cells
Adhesives
LCD and touch screens
Thin metals
Hard coatings
Biomedical coatings
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Polymer layers
Polymer web
SemiconSoft takes pride in building affordable, reliable and easy to use instruments for
measurement of thickness. SemiconSoft, Inc is the maker of MProbe thinfilm
measurement systems, Plasma Monitor system and TFCompanion software the de
facto software for thinfilm analysis.
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