Thin Film Measurement 1 Introduction In this lab you will use the phenomenon of interference and reflection to measure

the thickness of thin films. Two interference techniques, Michelson and Fizeau, will be studied and compared for accuracy, resolution and ease of use. The Michelson technique uses a Michelson interferometer with one of the mirrors replaced with the sample under test. The Fizeau technique uses a Fizeau interferometer to measure the shift in the interference pattern created between a Fizeau flat and the sample when they are held together with a minute air wedge between them. Both experiments require a step height in the film and the film and sample must be reflective. Another technique, which is used to measure thin film thickness without a step height in the film, is ellipsometry. This technique uses the change in polarization of the reflected light from the thin film and substrate interface to measure the film thickness. This process is more complicated and will also be demonstrated in this lab. The student should familiarize him/herself with the process before attempting this procedure. 2 Experimental Michelson Technique Two measuring techniques are used and compared with this set-up. The first involves using the micrometer on the mirror to measure the difference in zero path length between the thin film and no film. The second technique uses the step height change in the interference pattern much like the Fizeau technique. Set up the experiment as shown in Figure 1. The alignment of the set up is critical. All surfaces must be as close to perpendicular as possible. That is, the mirrors, cube beam splitter, and microscope objective faces must be perpendicular to each others normal. Place the DCX lens so that the image of the cube at the screen is focused and its largest, this is about 3.5 to 4 cm from the surface of the cube. Adjust the sample micrometer and microscope objective spacing so a bright focused spot of about 3 cm is seen on the screen through the beam splitter. Now adjust the mirrors thumb screws to centre the image from the objective inside the image of the cube beam splitter. An interference pattern should be seen within the image of the cube beam splitter. Adjust the sample stage position to come as close to zero path length as possible (you may have to adjust the position of the mirror so as not to change the size of the objective lens image too much), this will be apparent as the interference pattern becomes very large then becomes small again. Continue to adjust the mirror so the interference pattern is horizontally straight across the cube image. This is done by off-setting the interference pattern between two patterns, one at the top and one at the bottom of the cube image. See Figure 2 for a picture of the interference image required. Using the X and Y positioners on the sample stage, scan the wafer across the objective and stop when a resistor channel is found. Measure the width of this channel on the screen, compare this to the 20 u actual width and determine the magnification factor at the screen. Now without moving the Z position (you will change the magnification), move the sample using the X and Y micrometers until an image of a diode, capacitor, or resistor contact well is found. Position the vertical edge in -1

the middle of the interference pattern so it cuts the horizontal lines vertically in half. The interference image now is that of one through the oxide and one off the silicon substrate where the resistor contact pads were etched in the oxide.

Figure 1: Michelson interferometer to measure thin film thickness.

Figure 2: Interference pattern example. Measurement Now you have an interference pattern with a path length at the bottom of the well without an oxide layer and one with a path length through the oxide layer. Carefully adjust the mirror alignment so the lines are as parallel and horizontal as possible. Now move the mirror until zero path length for one side is achieved (this is when the lines are completely horizontal and maximumly spaced). Read the micrometer position. Now adjust the mirror position so the other side is at zero path length and read the new micrometer position. Calculate the oxide thickness using the following formula: (1) where noxide = 1.46 thickness = change in micrometer position (meters) magnification X n oxide

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Repeat this procedure a few times to ensure an accurate measurement. The measurement accuracy is based on the ability to find the zero path length for each side of the well. This zero path length point can be hard to determine so several measurements and then an average is needed. Can you suggest another way to optically detect zero path length difference? The second measuring technique for this set-up is the same as the Fizeau. By magnify the interference you should be able to see the fringes bend up or down and then run horizontal again (see fig 3). By physically measuring the step height and comparing it to the measured spacing between the fringes you can calculate the film thickness. Fizeau Technique The set up for this experiment is not much different from the Michelson set up. Block the mirror of the previous set up with a piece of paper. Remove the X40 microscope objective and replace with the X4 objective. Add the Fizeau flat between the objective and the sample and secure in place such that the sample can be brought into contact with its optically flat surface. See Figure 3 for set up configuration. Remove the silicon wafer from the sample stage and replace it with the aluminum coated glass slide with the graded step height. Now, using the Z micrometer, carefully move the glass slide against the Fizeau flat. Position the objective lens such that the image of the graded line on the sample is sharply focused, leave the objective in this position. By using the thumbscrews on the sample mount, you can adjust the air wedge such that an interference pattern of evenly spaced horizontal lines is achieved.

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Figure 3: Fizeau interferometer set-up.

Measurement The interference pattern should look like that of Figure 4. The graded step height in the thin film has produced a displacement of fringe lines, the amount of displacement represents the step height (i.e. film thickness). It is known that the distance between the interference lines is exactly half the wavelength of light used. In this case 6328 A/2 = 3164 A. Therefore, the film thickness is given by the formula: (2) film thickness ( ) = 3164
$

step height fringe spacing

The fringe spacing is the measured spacing on the screen between the interference lines and the step height is the measured space from one step of the step to bottom of the step following one of the fringe lines. Both these measurements would be made on the screen and would be given in millimeters.

Figure 4: Fizeau interference pattern Ellipsometry Refer to the operating procedures posted in the lab to set up the ellipsometer. Allow the mercury light to warm up for at least 10 minutes before proceeding with measurements (alignment can be performed during this time).

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Theory In order to electrically isolate various parts of an integrated circuit from one another, it is necessary to grow or deposit an insulating material between the active areas. This material could be an oxide of a few 100 to a few 1000 Angstroms in thickness. Determination of how much oxide has been formed requires a method which is nondestructive, since you don=t want to interfere with the integrated circuit structure, and yet be sensitive enough to give a close approximation of the films thickness. These specifications are met by the ellipsometer. Ellipsometry is the measure of reflections and their effect on the polarization of light. Such information gained from the measurements may be interpreted to yield the optical constants of the reflected material or, when the reflecting material is a film covered substrate, the thickness and optical constants of the film. What happens when light is reflected off a material? A planepolarized beam of light reflected off a surface can become elliptically polarized (see Figure 5). Figure 5: Plane polarized reflection

Ellipticity is a result of a phase change (small delta), between the Ap@ and the As@ components of the reflected light and a change in the ratio of their amplitudes, denoted as psi (see Figure 6), where (2) = arctan{R p / Rs Es / E p }

Figure 6: Relative -5

phase shift between

incident and reflected waves. This phase change varies for the various values of the incident angle phi and for different metals (see Figure 7). This phase angle change is referred to in ellipsometry as (capital) delta, defined as: (3)

s ) reflec ( p s )incident

Figure 7: Phase change vs. Incident angle for three different metals. The azimuth angle psi between the components R p and Rs , is a measure of the relative absorption of these two reflected components by the material.

Rp = tan Rs

Figure 8: Rp and Rs relation. The complete expression from a three dimensional point of view must take into consideration not only the value of psi, but also the phase change as well. Therefore, the complete formula becomes, Rp = (tan )(exp i ) Rs {absorbtion change} & {phase change} The operating principle of an ellipsometer is just the reverse of that phenomena described above. (4) -6

See Figure 9 for the basic components of an ellipsometer.

Figure 9: Ellipsometer set-up Collimated monochromatic light, normally of the mercury green line, (5460.73 A) is used. The polarizer, (a Glan-Thompson or a Nicol prism) is mounted in a graduated circle, serving to polarize the light emitted by the source. The compensator, is a birefringent plate usually of quarterwave thickness. It is used to convert the linearly polarized light into elliptically polarized light. Hence, the light incident upon the sample has an azimuthal angle psi and an ellipticity predictable from the polarizer and compensator settings. The azimuthal angle is determined by the analyzer located in the path of the reflected beam. Therefore, any change in the light=s ellipticity and azimuthal angle due to the reflectance from the sample is controllable. Any ellipticity existing in the light reaching the analyzer cannot be removed by adjusting the analyzer only. Both the polarizer and the compensator must be readjusted alternatively to remove this ellipticity. When this has been accomplished, the light reflected from the sample is plane polarized and can be readily extinguished by the adjustment of the analyzer. The use of a phototube and photometer increase the accuracy for determining the final settings of the compensator and analyzer for the points of extinction. The determination of capital delta and psi from the ellipsometer scale readings AP@ and AA@ are related (assuming a perfect quarter-wave plate for the compensator) by the equations: (5) and (6) = 1 2 2 P = - Ap = As

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There are, however, for any given surface a multiplicity of polarizer, analyzer and compensator scale settings that produce extinction making the determination of psi rather tedious. It is however possible to subdivide the determinants into four areas, (or what is commonly referred to in the literature as zones). Though the meaning of these zones will not be elaborated here, it is sufficient to remember that they are related to the values of AP@ and AA@ as follows: AP@ - the angle between the polarizer plane of transmission can be related to the surface of the material as being in either the plane of incidence, or the plane of the surface. AA@ - can be subdivided down into A As @ and Ap@according to whether AP@ is the angle between the polarizer plane of transmission and the plane of incidence or the materials surface plane. These relationships can be summarized as follows:

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The relationship between capital delta and psi and the optical parameters n, k and d of some film are expressed by the Fresnel reflection coefficients. This reflection coefficient is a ratio of the electric field vector Er of the reflected wave to that of the incident wave Ei , in terms of the amplitudes of both waves and the associated phase change due to the reflection, (7) r = (Er Ei )ei

The reflection of a wave of any polarization is given by the two coefficients Rp and Rs of the component waves. The ratio of these are, (8) rp rs = (Erp Ers ) (Eis Eip )ei (p s ) From the definition of capital delta and psi, given earlier, it follows that, (9) rp rs = tan ei The Fresnel reflection coefficients for a film-covered substrate are, (10) tan e =
i

rp 01 + rp12e 2 i 1 + rp 01rp12 e 2i

1 + rs 01rs12e 2 i rs 01 + rs12 e 2i

Therefore the complete equation for ellipsometry is, (11) + r12 e 2i r01 r = , where is p or s r12 e 2 i 1 + r01 The Fresnel reflection coefficients for a clean substrate are, (12) and (13) rsab = (na cos 1 nb cos 2 ) (na cos 1 + nb cos 2 ) where a and b represent the ambient medium and the substrate respectively. The phase change small delta can be determined from the equation, (14) rpab = (na cos 2 nb cos 1 ) (na cos 2 + nb cos 1 )

= (360 )d (n12 sin 2 )

12

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By substituting equations (12), (13), and (14) into equation (11), d can be determined as a function of capital delta, psi, angle of incidence, indices of refraction of the film and substrate and the wavelength of the light used. In doing this one must remember that n1 and n2 and the angle of reflection and refraction for an absorbing film and substrate will be complex, to say nothing of the calculation involved. In this lab we will use a table of values of small delta given for measured values of n1, capital delta, and psi for transparent films on silicon. The value of small delta can then be substituted into equation (14) along with n1 to calculate d.

Report Your report should include, along with your results and analysis of the accuracy, resolution and practicality of all techniques, a brief discussion of ellipsometry and other optical techniques for measuring thin film thickness. Be sure to include their advantages and disadvantages. Your report should also include a derivation of the magnification within one arm of the Michelson interferometer as it relates to the amplified displacement in the mirror arm (i.e., derive the formula used in the Michelson experiment). References [1] Lumdmila Eckertova, author, APhysics of Thin Films@, Plenum Press, 1986. [2] Theo Tschudi, chair, AThin Film Optics@, SPIE, 1989. [3] Leslie L. Ward, author, AThe Optical Constants of Bulk Material and Films@, A. Hilger, 1988. [4] Zden Knittel, author, AOptics of Thin Films@, Wiley, 1976.

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