Determination of the Mechanical Response of Thin Films with X-Rays

1993 ◽  
Vol 308 ◽  
Author(s):  
I. C. Noyan ◽  
G. Sheikh

ABSTRACTThe mechanical response of a specimen incorporating thin films is dictated by a combination of fundamental mechanical parameters such as Young's moduli of the individual layers, and by configurational parameters such as adhesion strength at the interface(s), residual stress distribution and other process dependent factors. In most systems, the overall response will be dominated by the properties of the (much thicker) substrate. Failure within the individual layers, on the other hand, is dependent on the local strain distributions and can not be predicted from the substrate values alone. To better understand the mechanical response of these systems, the strain within the individual layers of the thin film system must be measured and correlated with applied stresses. Phase selectivity of X-ray stress/strain analysis techniques is well suited for this purpose. In this paper, we will review the use of the traditional x-ray stress/strain analysis methods for the determination of the mechanical properties of thin film systems.

Author(s):  
D. R. Liu ◽  
S. S. Shinozaki ◽  
R. J. Baird

The epitaxially grown (GaAs)Ge thin film has been arousing much interest because it is one of metastable alloys of III-V compound semiconductors with germanium and a possible candidate in optoelectronic applications. It is important to be able to accurately determine the composition of the film, particularly whether or not the GaAs component is in stoichiometry, but x-ray energy dispersive analysis (EDS) cannot meet this need. The thickness of the film is usually about 0.5-1.5 μm. If Kα peaks are used for quantification, the accelerating voltage must be more than 10 kV in order for these peaks to be excited. Under this voltage, the generation depth of x-ray photons approaches 1 μm, as evidenced by a Monte Carlo simulation and actual x-ray intensity measurement as discussed below. If a lower voltage is used to reduce the generation depth, their L peaks have to be used. But these L peaks actually are merged as one big hump simply because the atomic numbers of these three elements are relatively small and close together, and the EDS energy resolution is limited.


Author(s):  
J N Chapman ◽  
W A P Nicholson

Energy dispersive x-ray microanalysis (EDX) is widely used for the quantitative determination of local composition in thin film specimens. Extraction of quantitative data is usually accomplished by relating the ratio of the number of atoms of two species A and B in the volume excited by the electron beam (nA/nB) to the corresponding ratio of detected characteristic photons (NA/NB) through the use of a k-factor. This leads to an expression of the form nA/nB = kAB NA/NB where kAB is a measure of the relative efficiency with which x-rays are generated and detected from the two species.Errors in thin film x-ray quantification can arise from uncertainties in both NA/NB and kAB. In addition to the inevitable statistical errors, particularly severe problems arise in accurately determining the former if (i) mass loss occurs during spectrum acquisition so that the composition changes as irradiation proceeds, (ii) the characteristic peak from one of the minority components of interest is overlapped by the much larger peak from a majority component, (iii) the measured ratio varies significantly with specimen thickness as a result of electron channeling, or (iv) varying absorption corrections are required due to photons generated at different points having to traverse different path lengths through specimens of irregular and unknown topography on their way to the detector.


1995 ◽  
Vol 20 (2) ◽  
pp. 125-177 ◽  
Author(s):  
I. C. Noyan ◽  
T. C. Huang ◽  
B. R. York

2016 ◽  
Vol 23 (3) ◽  
pp. 729-734 ◽  
Author(s):  
Roland Resel ◽  
Markus Bainschab ◽  
Alexander Pichler ◽  
Theo Dingemans ◽  
Clemens Simbrunner ◽  
...  

Dynamical scattering effects are observed in grazing-incidence X-ray diffraction experiments using an organic thin film of 2,2′:6′,2′′-ternaphthalene grown on oxidized silicon as substrate. Here, a splitting of all Bragg peaks in the out-of-plane direction (z-direction) has been observed, the magnitude of which depends both on the incidence angle of the primary beam and the out-of-plane angle of the scattered beam. The incident angle was varied between 0.09° and 0.25° for synchrotron radiation of 10.5 keV. This study reveals comparable intensities of the split peaks with a maximum for incidence angles close to the critical angle of total external reflection of the substrate. This observation is rationalized by two different scattering pathways resulting in diffraction peaks at different positions at the detector. In order to minimize the splitting, the data suggest either using incident angles well below the critical angle of total reflection or angles well above, which sufficiently attenuates the contributions from the second scattering path. This study highlights that the refraction of X-rays in (organic) thin films has to be corrected accordingly to allow for the determination of peak positions with sufficient accuracy. Based thereon, a reliable determination of the lattice constants becomes feasible, which is required for crystallographic structure solutions from thin films.


1990 ◽  
Vol 187 ◽  
Author(s):  
S. Raud ◽  
Quat T. Vu ◽  
M-A. Nicolet ◽  
G. A. Pollock ◽  
K. W. Mitchell ◽  
...  

AbstractWe study the properties of CuInSe2 thin films grown on glass and on Mo substrates. The investigation is carried out with X-ray diffraction, RBS, XTEM and SEM.CuInSe2/Mo contact stability is investigated after annealing at 600°C. RBS reveals that this treatment induces an interdiffusion between the metal and the chalcopyrite. To clarify this reaction, we have investigated the individual thin-film couples upon annealing. RBS and X-ray diffraction reveal insignificant interaction between Mo/Cu and Mo/In, but Se reacts with Mo.


1997 ◽  
Vol 505 ◽  
Author(s):  
G. Cornella ◽  
S. Lee ◽  
O. Kraft ◽  
W. D. Nix ◽  
J. C. Bravman

ABSTRACTX-ray strain analysis via Generalized Focusing Diffractometry (GFD) [1], and the concurrent need for accurate values of the unstrained lattice parameter, are discussed. A new method for determining the unstrained lattice parameter without knowledge of the elastic constants of the sample material is described. Stress measurements at varying temperatures, and extraction of the coefficient of thermal expansion from these measurements, are demonstrated for aluminum and gold films.


1971 ◽  
Vol 25 (4) ◽  
pp. 489-493
Author(s):  
James D. Nohe ◽  
David A. Green

Tantalum–aluminum thin film composition has been determined destructively by atomic absorption and nondestructively by x-ray fluorescence spectroscopy. Samples representing several compositions (20–80 at.% aluminum) and thicknesses (500–6000 Å) were sputtered on glass, graphite, and platinum substrates. The films were dissolved from the platinum substrates for the determination of aluminum by atomic absorption. The weights of tantalum per unit area obtained by difference using this destructive technique were applied to the same samples on glass substrates for correlation with nondestructive x-ray fluorescence measurements. A linear curve, which is free from enhancement and absorption effects, is obtained for tantalum. This curve relates the nondestructive fluorescence intensities to film weights (µg/cm2) of tantalum. The composition of the film is determined nondestructively by utilizing this curve and the total film weight which is obtained by weighing the substrate before and after sputtering. Alternately, composition may be determined destructively by atomic absorption utilizing films dissolved from platinum substrates


2011 ◽  
Vol 44 (2) ◽  
pp. 409-413 ◽  
Author(s):  
D. Faurie ◽  
P.-O. Renault ◽  
E. Le Bourhis ◽  
T. Chauveau ◽  
O. Castelnau ◽  
...  

The anisotropic elastic response of supported thin films with a {111} fiber texture has been studied using anin-situmicro-tensile tester and X-ray diffractometry. It is shown which specific X-ray diffraction measurement geometries can be used to analyze the elastic strains in thin films without requiring any assumptions regarding elastic interactions between grains. It is evidenced (theoretically and experimentally) that the combination of two specific geometries leads to a simple linear relationship between the measured strains and the geometrical variable sin2ψ, avoiding the transition scale models. The linear fit of the experimental data allows a direct determination of the relationship between the three single-crystal elastic compliances or a direct determination of theS44single-crystal elastic compliance and the combination ofS11+ 2S12if the macroscopic stress is known. This methodology has been applied to a model system,i.e.gold film for which no size effect is expected, deposited on polyimide substrate, and it was found thatS44= 23.2 TPa−1andS11+ 2S12= 1.9 TPa−1, in good accordance with values for large crystals of gold.


1973 ◽  
Vol 17 ◽  
pp. 571-583
Author(s):  
R. P. Larsen ◽  
J. O. Karttunen

AbstractAn energy-dispersive X-ray spectrometer that (1) uses as the primary excitation source the power supply and tungsten X-ray tube from a conventional crystal spectrometer (General Electric XRD-6) and (2) uses as the secondary excitation source elemental metal foils that are readily interchangeable has been built and operated. The use of an X-ray tube with a high-voltage capability, 75 kilovolts max, enables the determination of elements with atomic numbers as high as 66 (terbium) to be based on the K series of X-rays; the highpower capability, 3.7 kilowatts max, enables a particularly intense beam of X-rays to be generated by the secondary source and hence, provides a particularly high detection capability for trace elements in a sample. An instrument that uses interchangeable secondary sources to irradiate the samples has several advantages over those instruments in which excitation is accomplished by direct irradiation with an X-ray tube: (1) the background radiation in the energy range where the X-rays of interest are measured is several orders of magnitude lower and is very uniform and (2) the energy of the excitation radiation can be closely matched to the absorption edges of the elements of interest in the sample.In the application of the instrument, particular emphasis has been placed on the development of tectmiques that will enable an energy-dispersive X-ray spectrometer to be used as the detection instrument for quantitative elemental analysis. Methods for the determination of the individual rare earths, plutonium and uranium at the microgram level with an accuracy of ± 1% are outlined and for the determination of plutonium and uranium at the milligram level with an accuracy of ± 0.1% are proposed.


1987 ◽  
Vol 31 ◽  
pp. 175-180
Author(s):  
James E. Willis

The use of empirical analysis techniques for the simultaneous determination of the thickness and composition of thin film samples usually requires a suite of well characterized similar type standards. While this may be adequate for a quality control application, this requirement severely limits the utility of X-ray fluorescence in the analysis of thin films in a service lab or research environment.The use of fundamental parameters in the analysis of thin films allows the simultaneous determination of the thickness and composition of single and multiple layer thin film unknown samples without the use of similar type standards.


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