Depth Profiling Biaxial Stresses in Sputter Deposited Molybdenum Films; Use of the Cos2φ Method

1995 ◽  
Vol 39 ◽  
pp. 363-370
Author(s):  
B. L. Ballard ◽  
P. K. Predecki ◽  
T. R. Watkins ◽  
K. J. Kozaczek ◽  
D. N. Braski ◽  
...  

Depth profiles of intrinsic in-plane, biaxial stresses were obtained as a function of τ, the 1/e penetration depth, in a 1.0 um thick planar d. c. magentron sputter deposited molybdenum film using asymmetric grazing incidence x-ray diffraction (GIXD). τ was varied between 20 and 276 Å. The stresses σ11 and σ22 were characterized in the directions parallel and perpendicular to the long axis of the cathode respectively using a cos2φ method. The results show that starting from τ=17Å, σ11 and σ22 are compressive and become rapidly more compressive with a minimum at τ ∼ 20 - 40 Å thereafter increasing gradually toward tensile values. The reasons for the shape of the stress gradient are not well understood but may be related to the relaxation of the stresses at the tops of the columnar Zone T-type microstructure and to the oxygen gradient in the film.

2006 ◽  
Vol 524-525 ◽  
pp. 13-18 ◽  
Author(s):  
A. Kumar ◽  
U. Welzel ◽  
M. Wohlschlögel ◽  
W. Baumann ◽  
Eric J. Mittemeijer

A rigorous strategy for (X-ray) diffraction stress measurements at fixed penetration/information depths is described. Thereby errors caused by lack of penetration-depth control in traditional (X-ray) diffraction (sin2ψ) measurements are annulled. The ranges of accessible penetration/information depths and experimental aspects are briefly discussed. The power of the method is illustrated by the analysis of an only small stress gradient in a sputter-deposited nickel layer.


1997 ◽  
Vol 504 ◽  
Author(s):  
M. Soltani-Farshi ◽  
H. Baumann ◽  
D. Rück ◽  
G. Walter ◽  
K. Bethge

ABSTRACTThe influence of nitrogen ion implantation on the hydrogen accumulation in titanium was investigated as function of sample temperature and ion fluence. 150 keV nitrogen (15N) ions were implanted at different sample temperatures up to 700°C with fluences ranging from 1 × 1017 to 1 × 1018 ions/cm2. The amount of accumulated hydrogen and its depth distribution was measured quantitatively with the 15N depth profiling method. The implanted 15N depth profiles were measured by the reverse reaction 15N(p, αγ)12C at 429 keV. The binary phases of the implanted nitrogen with titanium are detected by grazing incidence x-ray diffraction. The results are compared with those obtained for samples implanted at RT and subsequently thermally treated.


2003 ◽  
Vol 763 ◽  
Author(s):  
I.M. Kötschau ◽  
G. Bilger ◽  
H.W. Schock

AbstractGrazing incidence X-ray diffraction (GIXRD) in conjunction with a layer absorption modeling algorithm is a powerful tool for studying the structural properties of polycrystaline thin films. A typical application is the refinement of compositional depth profiles. Of genera interest are the depth profile of the Ga/(In+Ga)-ratio over the entire thickness of the thin film, as well as the depth profile of th Cu/(In+Ga)-ratio near the surface. In this respect the three stage process is a particular interesting deposition technique. A remarkable recrystalization of the entire thin film at the end of the second stage has a strong impact on Ga-gradients as well as on the Cu-depletion close to the surface. In this contribution we use the GIXRD technique to refine composititional depth profiles obtained by secondary ion mass spectrometry (SIMS). We demonstrate that structura changes near the surface due to the recrystalization can be monitored. In addition we are able measure the depth of a Cu-depleted surface layer with high accuracy.


1992 ◽  
Vol 36 ◽  
pp. 237-245 ◽  
Author(s):  
Paul Predecki ◽  
X. Zhu ◽  
B. Ballard

AbstractTwo proposed methods are described for obtaining the depth profiles (τ-profiles) of strains and stresses as a function of the 1/e penetration depth τ, using GIXD in the asymmetric geometry, without the need for layer removal. In the first, the ψ-method: ψ is varied, for a given reflection, while holding τ constant, by varying the wavelength λ and adjusting the incident angle α so as to maintain τ constant. This allows dϕ,ψ vs Sin2ψ plots to be obtained at constant τ. In the second, the ϕ-integral method: interplanar spacings dϕ,ψ are measured for ϕ values from 0 to 2π, at constant ψ and τ by holding α fixed. Two ψ values, i.e. two wavelengths, are needed to obtain the whole strain tensor, but if the sample is quasi-isotropic and the stress state is biaxial, only one wavelength is needed. A direct method is also described for obtaining the profiles as a function of depth z (z-profiles) from the corresponding τ-profiles using inverse Laplace transforms. Application of the method to the residual strain vs τ data of Doerner and Brennan for an Al film on Si is presented.


2006 ◽  
Vol 514-516 ◽  
pp. 1618-1622 ◽  
Author(s):  
Maria José Marques ◽  
J.C.P. Pina ◽  
A. Morão Dias

The conventional Bragg diffraction geometry, normally used to characterize the residual surface stress state, it is not suitable to evaluate surface treated materials and thin films. The X-ray path lengths through a surface layer or thin film are too short to produce adequate diffraction intensities in relation to the bulk or the substrate. Another limitation of the conventional technique appears when a residual stress gradient is present in the irradiated surface. The technique only enables the evaluation of the mean value of this gradient. In these cases, a recently proposed Pseudo-Grazing Incident X-ray Diffraction method would be better applicable. In this study, the Pseudo-Grazing Incidence X-ray Diffraction is applied to characterize the residual stress depth profiles of several AISI 4140 samples, which were prepared, by mechanical polishing and grinding, in order to present different surface roughness parameters, Ra. The experimental results lead to the conclusion that the surface roughness limits the application of the Pseudo-Grazing Incidence methodology to a minimum X-ray incident angle. This angle is the one that enables a mean X-ray penetration depth with the same order of magnitude of the sample surface roughness parameter, Ra.


1987 ◽  
Vol 2 (4) ◽  
pp. 471-477 ◽  
Author(s):  
G. Lim ◽  
W. Parrish ◽  
C. Ortiz ◽  
M. Bellotto ◽  
M. Hart

A method using synchrotron radiation parallel beam x-ray optics with a small incidence angle α on the specimen and 2Θ-detector scanning is described for depth profiling analysis of thin films. The instrumentation is the same as used for Θ:2Θ synchrotron parallel beam powder diffractometry, except that the specimen is uncoupled from the detector. There is no profile distortion. Below the critical angle for total reflection αc, the top tens of Angstroms are sampled. Depth profiling is controlled to a few Angstroms using a small α and 0.005° steps. The penetration depth increases to several hundred Angstroms as α approaches αc. Above αc there is a rapid increase in penetration depth to a thousand Angstroms or more and the profiling cannot be sensitively controlled. At grazing incidence the peaks are shifted several tenths of a degree by the x-ray refraction and an experimental procedure for calculating the shifts is described. The method is illustrated with an analysis of iron oxide films.


1993 ◽  
Vol 37 ◽  
pp. 197-203 ◽  
Author(s):  
Xiaojing Zhu ◽  
Paul Predecki

AbstractA numerical procedure is described and demonstrated for determining z-profiles from measured τ-profiles of diffraction data such as may be obtained by grazing incidence x-ray diffraction (GIXD). The z-profile was approximated by a piece wise linear function and the problem of solving the integral equation for the z-profile was thus converted to one of solving a set of linear equations. With a sufficient number of the linear pieces, the z-pTofile could be accurately determined. The procedure and its sensitivity to data errors was tested with several arbitrarily chosen known functions. It was found that when errors were introduced into either the τ-profile or the sample thickness D the resulting z-profiles become oscillatory.


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