Null

Ellipsometry: A Basic Experimental Procedure

Submitted to:

Dr. Stephen Ducharme Professor of Physics University of Nebraska-Lincoln

Submitted on:

May 5, 2010
Submitted by:

Jeremy VanDerslice

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Purpose
To learn the fundamentals of null ellipsometry

Introduction
Ellipsometry is an extremely sensitive technique used to analyze the properties of surfaces or thin films. Ellipsometry can be used to find the index of refraction, extinction coefficient, reflectivity, or thickness of a surface or thin film, among other things. In basic terms, ellipsometry measures the change in polarization that occurs as light is reflected off of a target surface. With this in mind, ellipsometry could very well be called polarimetry except that a differing technique not related to ellipsometry was already coined polarimetry. Although it can be disputed who actually invented ellipsometry, Paul Drude derived the fundamental equations of ellipsometry in the early 1900s and based on his work Alexander Rother then coined the term ellipsometry in a journal article in 1945. The name stems from the fact that the most basic form of polarized light is elliptic. [1]

General Ellipsometry Theory

Snells Law To define the general equation of ellipsometry, many key definitions must first be discussed. First, incident light transmitted and reflected at a medium is defined to act in a plane of incidence. The plane of incidence is shown in Figure 1.

Figure 1. Incident, reflected, and transmitted light in the plane of incidence. [1]
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Snells law defines how light interacts with a medium as it passes through it. Snells relates the complex index of refraction to the angles of incidence of the medium. The index of refraction is a complex argument defined by: =+ Where n relates the speed of light in the medium to the speed of light in a vacuum, = . The extinction coefficient, k, is defined through the absorption coefficient () which describes how quickly the amplitude of the light wave decreases as it travels through a medium, =, , =4 Thus, Snells law can be properly described by the following equation, 11=22 Where 1 is the angle of incidence measured from the boundary unit normal and 2 is the angle of transmission also measured from the unit normal. For a dielectric material in which no light is absorbed the complex portion of the argument is zero, thus, for this simplified case, Snells law can be expressed as, 11=22 However, for the sake of this deriving the general ellipsometry equations only the most general case will be considered. Fresnels Equations Ellipsometry investigates the phase change of these components when reflected off a surface. In general the phase change is not the same for both components and the result is elliptically polarized light. The elliptically polarized light can be defined by two components, p-wave and s-wave. The p-waves is defined as the polarized wave parallel to the plane of incidence while s-wave is defined as plane polarized wave perpendicular to the plane of incidence. Fresnel reflection coefficients define the amplitude change between the incident and reflected waves at an interface. They are defined by the following expression, 12=211221+12 12=112211+22 Where 1 and 2 are shown in Figure 2. Azzam furthered the understanding of the Fresnel reflection coefficients by defining how the amplitude between the incident and reflected waves change when thin films are present. He defined an optical thickness as the distance the waves travel through the thin film and then integrated these findings to with the Fresnel reflection coefficients as follows,
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=12+2321+12232 =12+2321+12232 , =222 Where is the optical thickness, d is the thickness of the thin film, and is the wavelength of the light source.

Figure 2. Reflection and transmission of light at thin film boundary. [2] General Ellipsometry Equation Incident light reflecting off a surface undergoes a change in phase. Let 1 describe the phase difference between the s- and p-waves for the incident light and 2 describe the phase difference between the s- and p-waves for the reflected light. Now, let describe the change in phase between the parallel and perpendicular components of the incident light that occurs when it is reflected from a surface, =12 As previously discussed, the Fresnel equations define amplitude ratios and can be used define the change of amplitude of the light waves as they are reflected, = A new term, , has been introduced to quantify the amplitude change that occurs upon reflection. Using the previous definitions, the fundamental equation of ellipsometry can now defined as, = Thus, the thickness and complex refraction of a thin film can be found if the complex refraction of the substrate and the outside environment (usually air) are known. [2]
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Null Ellipsometry
The previous derivation of the fundamental equations of ellipsometry is valid for all types of ellipsometry. However, in this experiment only null ellipsometry will be investigated. Null ellipsometry is one of the oldest forms of ellipsometry and it is still one of the most accurate, even when done manually. However, it is often very slow and the calculations required to extract and can be very tedious when done by hand. The typical setup of a null ellipsometer is shown in Figure 3. It is known as the PCSA configuration or polarizer-compensator-sample-analyzer configuration. There are many different ways to setup a null ellipsometer, including PSCA and PSA, but PCSA is the most common. The PCSA configuration can be used fairly simply to obtain the two ellipsometric parameters for the sample. The basic procedure consists of finding component settings that extinguish the light at the detector. The azimuths of the polarizer and compensator (Po & Co) are adjusted to make the elliptically polarized light reflect off the sample as linearly polarized light. The reflected light is then extinguished by a suitable analyzer angle, Ao. Assuming the light is completely extinguished, the complex reflectance ratio can be defined as =ctanPoCo+tanCotanPoCotanCo1tanAo = Where the transmittance ratio of the compensator is denoted by c. It is evident that this is a fairly complex equation but in this investigation a simplification will be used in which the compensator will be held constant at a quarter-wave, Co=/4. With this simplification it is known that the reflected light can be extinguished with two different settings P1 and A1, and P2 and A2. These settings are known to be related to each other by P2=P1 and A2=-A1. In addition, these measurements are related to the ellipsometric angles by, =1 =21+32 10 (1) =1 =21+2 1<0 (2) This form of ellipsometry is usually done at various angles of incidence. The location in which the minimum polarizer setting occurs will be used to calculate the ellipsometric angles for this investigation. This is due to the fact that the minimum is usually at or near Brewsters angle and it is at this location that the most pronounced changes in polarization will occur, thus being most easily measured. This location is called the principal angle of incidence. The corresponding analyzer angle is called the principal angle of azimuth. [3]

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Figure 3. Polarizer-Compensator-Sample-Analyzer configuration of a null ellipsometer. [3] Once the ellipsometric angles are known, the extinction coefficient, index of refraction and reflectivity of the sample can be calculated from Drudes approximation equations [4] =tan2 (3) =2212 (4) =(1)2+22(+1)2+22 (5)

Experimental Procedures
Equipment The following equipment will be used for this experiment: High pressure mercury lamp, 5461 green line filter, Gaertner spectrometer, rails, adjustable sample mount, polarizer, analyzer, Soliel-Babinet compensator, Gaussian eyepiece, photomultiplier tube, picoammeter, acetone, methanol, and a crystalline silicon wafer. Setup and Calibration: Fasten sample to Gaertner Spectrometer table using optical plate mount, rails, and adjustable sample mount. Place high pressure mercury lamp with filter at the collimator slit. Using the Gaussian eyepiece, adjust the telescope on the Gaertner Spectrometer until the cross-hairs are centered horizontally and vertically on the illuminated green rectangle produced by the slit on the collimator. Adjust the vertical tilt on the telescope if needed. Turn the lower rotatable table, shown in Figure 4, until the 0o line matches up with the 180o line of the telescope. Place the sample on the adjustable sample mount that

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was constructed. Carefully clean the sample surface with acetone and then methanol to remove organic buildup. Slowly slide the sample along the rail until it is centered between the collimator and telescope. Analyzer Compensator Polarizer Adjustable Slit

Collimator

Lower Rotatable Table Upper Rotatable Table

Telescope

Photomultiplier Tube

Figure 4. Essential components of PCSA null ellipsometry with Gaertner Spectrometer. Place the polarizer on the end of the collimator and set it to 0o. Adjust the telescope to silicons Brewster Angle (angle of incidence of 152.6o).Rotate the entire polarizer (while keeping the polarizer set to 0o) until the photomultiplier tube detects a minimum amount of light. The polarizer is now known to be oriented such that the 0o setting produces light polarized vertically. Now, set the angle of incidence to 0o and place the analyzer on the end of the telescope and set it orthogonal to the polarizer. Rotate the entire analyzer (while keeping it orthogonal to the polarizer) until maximum extinction is found and tighten it down. Attach the compensator to the spectrometer. With the polarizer at +45o and the analyzer at -45o, rotate the compensator until maximum extinction is found. Adjust the retardation on the compensator by turning the knob to correspond with a quarter wave phase shift (1.33 turns) as given by Table 1.
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Table 1. Soliel-Babinet calibration guide to set the retardance of the compensator. Note k=0.987 [Appendix B] Procedure Set the angle of incidence to 170o by rotating the telescope. Next, rotate the polarizer until maximum extinction is found. Then, adjust the analyzer to further reduce the signal produced by the photomultiplier tube. Continue to adjust the analyzer and polarizer until the maximum extinction is found. Record the polarizer and analyzer azimuth settings. Next, adjust the polarizer and analyzer to allow for maximum transmission. Now, adjust analyzer for maximum extinction and then sequentially adjust the polarizer and analyzer for maximum extinction. If the azimuths of the analyzer and polarizer are different than the first measurement, record the values. If they are the same, adjust the polarizer to a new location and begin again by adjusting the analyzer for maximum extinction. Once both null positions are found, reduce the angle of incidence by 10o and repeat measurements for angles of incidence between 170o and 60o at 10o increments. Sort the data into two consistent data sets and plot the polarizer and analyzer angles as a function of angle of incidence. References and Additional Reading [1 ] Santer, S. (2004, July 20). Ellipsometry. Retrieved from http://www.imtek.de/cpi/images/images/vl- ofa/OFA-elli.pdf [2] Tompkins, Harland, & McGahan, William. (1999). Spectroscopic ellipsometry and reflectometry. New York: Wiley-Interscience [3] Tompkins, Harland, & Irene, Eugene. (2005). Handbook of ellipsometry. William Andrew. [4] Monk, G.S. . (1963). Light: principles and experiments. New York: Dover Publications. [5] Azzam, R., & Bashara, N. (1987). Ellipsometry and polarized light. North Holland. *See Appendix for critical information about Gaertner Null Ellipsometer Equipment
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Comments for Dr. Ducharme Following the procedure that was previously outlined, raw data was collected as shown in Table 2. The data can be compared to the expected results remembering that the two null positions for each angle of incidence should have the following relationship, P2=P1 and A2=-A1. It is quickly evident that the raw data collected doesnt directly follow the guideline. 2 Null 1 Null 2

Analyzer Polarizer Analyzer Polarizer

170 85 62 41 66 51 165 82.5 75 54 160 80 74 31 82 60 155 77.5 80 22 88 79 152 76 79 3 88 90 150 75 78 7 88 79 145 72.5 74 24 88 73 140 70 72 32 82 61 130 65 67 37 74 51 Table 2. Raw data collected from analyzer and polarizer azimuth measurements The raw data shows that 1!2 and 2!901. The analyzer azimuth measurement is the complementary angle to the one that is desired thus, 1=901. After making the adjustment, 2=901 and 2=901 so the relationship between the two null sets of the measured data is slightly different than that given by H. Tompkins. This discrepancy is still under consideration, but it is thought that the difference has something to do with the scale on the polarizers. Although the adjustments are simple, the changes are made and shown in Table 3 for clarity. 2 Null 1 Null 2

Analyzer Polarizer Analyzer Polarizer

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170 85 28 41 -66 -51 165 82.5 -75 -54 160 80 16 31 -82 -60 155 77.5 10 22 -88 -79 152 76 11 3 -88 -90 150 75 12 7 -88 -79 145 72.5 16 24 -88 -73 140 70 18 32 -82 -61 130 65 23 37 -74 -51 Table 3. Data after modifications are made to prepare them for use in ellipsometric equations The analyzer and polarizer azimuth measurements are plotted as a function of angle of incidence in Figure 5. Notice that the principal angle of incidence is located at the dip in the curves. The azimuth measurement of the analyzer at this location is the principal angle of azimuth. This is the location and measurement that will be used later in calculations.

50 Polarizer , Analyzer [deg] 30 10 -10 -30 -50 -70 -90 65 Angle of Incidence [deg] 70 75 80 85 Null 1 - A Null 1 - P Null 2 - A Null 2 - P

Figure 5. Analyzer and polarizer adjusted azimuth measurements as a function of the angle of incidence. Now, the extinction coefficient, index of refraction, and reflectivity can be extracted from the data using equations (3), (4) & (5). Although it seems that any angle of incidence could be used to extract these properties, the angle of incidence nearest to Brewsters angle is chosen because it provides the greatest change in polarization so the measurement can be found with less error. The calculated extinction coefficient, index of refraction, and Reflectivity are compared to values given by the SOPRA N&K Database in Table 4.

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SOPRA N&K Database 0.0415 4.099

Measured: Null location 1 0.404 4.254 0.452

Rel. Error 10x 3.8% 15.3%

Measured: Null Location II 0.067 3.901 .400

Rel. Error 68% 4.8% 1.9%

k n

R .392

Table 4. Extinction coefficient (k), Index of Refraction (n) and Reflectivity (R) as given by the SOPRA N&K database in comparison to values calculated from measurements. The relative error in the calculated extinction coefficients immediately draws concern. However, it was found that the extinction coefficient is extremely sensitive to the azimuth of the analyzer. For instance, the Null 2 analyzer azimuth reading at the principal angle of incidence is -88o, which leads to an error of 68%. If the reading would have been only 1o different (-89o) the error would have only been 15%. Even though the index of refraction and reflectivity are function of the extinction coefficient, the dependence is weak. The huge reduction of error (concerning the hypothetical case that =-89o rather than -88o) in the extinction coefficient only improves the error in the index of refraction by 0.2% and the error in the reflectivity by 1.4%. This explains how the index of refraction and reflectivity for the Null 1 data set are reasonably close to accepted values even though the extinction coefficient is off by 1000%. Throughout the experiment it was found that obtaining precise measurements with the polarizer and analyzer is fairly difficult leading to much less precision in the null ellipsometry experiment than advertised in literature. When reading through some literature on null ellipsometry, it was found that a manual null ellipsometer typically use polarizers that are accurate within 0.01o. The polarizers used in this experiment were accurate to 0.5o while actually achieving this accuracy was often difficult. With patience it was found that the tolerance on the azimuth measurements was no less than 2.5o. Even with this lack of precision, values were obtained that compared reasonably well to accepted values.
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Conclusion (Personal Notes): My method for finding both null positions for each angle of incidence is not an exact science; however, it seemed that the order in which the polarizer and analyzer were adjusted could influence the null position that was found. This is the procedure I outlined, but I admit that it didnt always work well for me. Im slightly perplexed by a few things in the raw data, namely, the relationship between the two null sets. I found the theoretical relationship given by Tompkins doesnt directly match what I have. I often saw in the literature that people use an analyzer that has a range of -180o to 180o and a polarizer that has a range from 0o to 360o. The polarizer and analyzer that I used ranged from 0o to 90o. I think this difference in scale camouflages my data to look different than what Tompkins predicts while it is actually the same. Overall, this was a fairly comprehensive experiment covering a range of things that were learned during the lab but it really helped to solidify the concepts we learned during the polarization experiment. Assuming that Ive explained my procedure well enough to reproduce, I think this entire experiment could be easily duplicated in a 2-week lab, the first week probably being setup and calibration and the second week data collection. Comments on the Class The class was both interesting and challenging. I really appreciated the fact that it is taught by a professor rather than a TA, which is so often seen in the engineering college. You brought a lot of enthusiasm about the subject to the class and that made working a little harder to learn things a lot easier. Thanks for the extra time you spent helping me get this extra experiment going as well as all the rest. Have a good summer. Regards, Jeremy

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Appendix

Introduction to Lasers and Modern Optics University of Nebraska Lincoln Jeremy VanDerslice