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.

The composition of ancient Chinese bronze mirrors has been determined by X-ray fluorescence measurements. The mirrors were archived to be from either 200 BCE-200 CE and from approximately the 800 CE period. Glancing incidence X-Ray excitation proofed highly useful for obtaining the elemental composition from the fluorescence measurements. Measurements of the tin L/K X-ray fluorescence ratio as a function of the glancing incidence angle showed that this ratio became independent of the glancing angle for angles less than 5°. Glancing X-ray fluorescence measurements made at 2° were then calibrated to known standards to give highly accurate compositions for major elements in the Chinese bronze mirrors. X-Ray diffraction measurements were used to test for composition segregation or crystal structure changes near the surface of the mirrors. The X-ray diffraction angles were found to be independent of the glancing angle indicating that surface composition segregation was not observed. Changing relative intensities of the observed diffraction reflections indicated that the crystal texturing changed near the surface.

A method has been developed for the determination of the amorphous content of superconducting films (niobium-germanium) based on x-ray analysis. Measurements are made in reflection using a standard diffractometer which includes a silicon semiconductor counter. The intensity of the diffraction line of the substrate was measured at an angle outside the amorphous halo region of the films to calibrate their surface density. The second angle of measurement was chosen to be within the region of the amorphous halo but away from the diffraction lines of the substrate or crystalline components of the films under investigation. Expression have been derived for calculation of the amorphous content. For the set of films investigated, a direct correlation of the amorphous concentration and the superconducting transition temperature has been observed.

Traditionally, in X-ray fluorescence analysis for the determination of elemental compositions, the fluorescence is measured from the irradiated side of the sample. The composition measurements obtained by this method are sensitive to a gradient in composition as a function of depth of the element being measured. This report presents a simple method for measuring a mean composition for an element segregated in layers applicable to thin samples so that the fluorescence can be measured on the side opposite to that being irradiated. It is shown that for a particular relation between the angle of incidence of the primary radiation and of the detection angle on the opposite side of the sample that a mean concentration can be measured for an element which is independent of the composition in the separate layers.

This paper presents a nondestructive measurement technique for the accurate and absolute determination of film thicknesses of Co and SmCo based magnetic films deposited by sputtering on single crystal Silicon (100) substrates. X-Ray diffraction of Cu K 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 4-axis research diffractometer allowed the substrate orientation to be fine adjusted to maximize the (400) diffraction intensity. The absolute thickness of SmCo based films was in a range from 0.05 to 5 Co film thicknesses on Si could be measured to a few tens of nanometers. The absolute accuracy of the thickness measurements depend on the effective mass attenuation coefficient of the film material. For the materials considered, thicknesses determined by the X-Ray attenuation method agree within at least several percent to values determined by other methods.