The thicknesses and oxygen concentration of tantalum oxide (TaO) and hafnium oxide (HfO) films, prepared by magnetron sputtering Ta and Hf in oxygen onto heated silicon (100) substrates, were measured by three different techniques. The first method uses X-ray reflectivity, which yields a thickness value independent of the film composition. The second method uses the simultaneous measurement of Ta and Hf fluorescence counts. For these <200-nm-thick films there is very little matrix effect so that the Ta and Hf fluorescence counts are expected to, and are observed to, increase linearly with the film thickness. The third method uses the attenuation of the Si Kα X-ray line from the underlying Si excited by a glancing incident X-ray beam for measurement. The TaO and HfO films were observed to grow for the sputtering conditions employed, in an initial mode characterized by a high mass absorption times density product and then grow as characterized by a lower mass absorption times density product. This change over occurred for the HfO films, at a film thickness of 13 nm. The change over occurred for the TaO films at a film thickness of 23 nm. Pure Ta and Hf films were also made by magnetron sputtering from Ta and Hf targets in argon. All X-ray measurements, including the reflectivity measurements, were made, with the addition of an X-ray fluorescence detector, using a Panalytical MRD system.

This paper presents a nondestructive measurement technique for the determination of the film thicknesses of Co and SmCo based magnetic films deposited by sputtering on single-crystal silicon (100) substrates. X-ray diffraction of Cu Kα radiation has been used to measure the intensity of the (400) reflection from bare silicon substrates and as attenuated by sputter coated Co and SmCo based films on Si substrates. A four-axis research diffractometer allowed the substrate orientation to be fine adjusted to maximize the (400) diffraction intensity. The thickness of SmCo based films was in a range from 0.05 to 5 μm. Co film thicknesses on Si could be measured to a few tens of nanometers. The accuracy of the thickness measurements depends on the effective mass attenuation coefficient of the film material. For the materials considered, the thicknesses determined by the X-ray attenuation method agree within at least several percent to values determined by other methods.