 the diffusion energy ED [eV], and on the temperature of the sample TS [K].
Challenges and improvements
The resolutions of high end SEMs drastically increased during the last years, what leads to new upcoming problems. One of them is that previously used preparation methods are at their limits. The conductive layer has to fulfil more requirements at high magnifications than for magnifications which are used for investigations by using conventional SEMs.
An example of a thin gold palladium film is shown in Figure 3.
At high magnification thin films show a structured surface which is not applicable for high resolution. The ditches which can be seen in Figure 3 (right) leads to a higher surface resistivity. This causes drifts and charging effects during image acquisition by high magnification. Therefore the morphology of thin films has to be improved for using it.
Characterisation of the device
Before the sputter coater is optimised for high resolution applications, the verification of the local temperature increase on the sample is varied. Especially the heat impact on the sample is important for a lot of nonconductive samples because even perfectly formed layers are useless if the surface is modified by the temperature. For these measurements a thermocouple is located on a model sample to monitor the temperature during the sputter process. Figure 4 shows the local temperature increase by increasing the current (upper) and the working distance (lower graph).
The graph below shows the comparison between the maximal and minimal working distance (WD) and it can be seen that the WD at the highest level leads to a sputter process which causes nearly no local temperature increase.
Besides the local temperature increase at the sample, the thickness values which are displayed during the sputter process were verified to check how precisely thin films are sputtered by Leica Microsystems’ sputter coater. Therefore, a multilayer system with different thickness values is sputtered which consists of two different materials. In this case, gold (Au) and tungsten (W) are used because the difference of the atomic number is adequate to get a good material contrast by the following TEM investigations.
Another reason to choose these target materials was the fact that the characteristic x-ray peaks, which have the highest intensities, do not overlap and an EDX line scan can be performed through the multilayer system. Out of the EDX line scan the thickness values can be measured and compared by the result of the built-in quartz. The results can be seen in Table 1.
|Material||dLeica [nm]||dmeasured [nm]||dmeasured – dLeica [%]|
Tab. 1: Comparison of the measured thickness and the expectation value. dLeica = setted thickness, whereat the sputter process will stop in nm; dmeasured = arithmetic averaged thickness value of all measurement methods in nm; dmeasured – dLeica = difference between expectation value and measured value in %.
Improvement of the sputtered films
To get a smooth and even surface, the sputter parameters which have the most influence on the film growth are systematically varied.
Thickness, working distance, current and argon pressure are changed in a certain range. The effect on the morphology by changing these parameters is more precisely described in . The most important parameter which changes the morphology of the thin film is the argon pressure in the chamber of the coater. A decreasing of the argon pressure to values below 1e–2 mbar leads to a even film abruptly. This behaviour was observed for different target materials and it was shown that this effect is independent of the used target and also the critical argon pressure is nearly the same for every material.
To understand the physics behind the formation of the even film by sputtering at lower argon pressure, the film growth of a thin film which is sputtered with ditches and without ditches was compared and observed by TEM investigations (see Figure 6). Based on these findings the sputtered layer must be at least 2 nm thick to get an even film and the growth of thin fil