We report the results of a recent study where nickel substrates electroplated with chromium were loaded in-situ on an x-ray diffractometer. This technique allows determination of lattice spacings in the vicinity of the interface for both the film and the substrate as a function of the applied load. We used such lattice parameter data, SEM observations of the surface and x-ray peak breadth data to study the partitioning of deformation between the film and the substrate. The data indicates progressive loss of adhesion between the film and the substrate with increasing deformation. We observe significant effect of electroplating residual stresses on the mechanical behavior of the system. The loss of adhesion between the film and the substrate coupled with the initial residual stress profile causes an apparent 'negative Poisson's ratio' for the film during initial stages of the loading. This effect disappears with cyclic loading and unloading.

Zn-Ni-alloy electroplated steels are one of the surface-treated materials with a high corrosion resistance and are mostly used for automobiles. It is said that the corrosion resistance is more than four times as great as that of Zn-plated steels. Concerning x-ray stress measurement, Kyono et al reported the result of measurement on y (552) planes and showed that the sin2φ diagram was severely curved.

X-ray stress analysis in surface-treated materials will become more important. Some problems, however, remain to be studied when we apply the x-ray method to thin layers. For example, the effective x-ray penetration depth may be different from that in ordinary materials. And complex gradients of stresses and compositions may exist.

Thin film metallization is used on integrated circuit chips and ceramic and/or organic substrates for a number of different purposes, On chips the metallization forms Ohmic and Schottky Barrier Diode contact to the semiconductor and the electrical properties of these contacts are strongly influenced by the metals used. Interaction of the metal and semiconductor during processing can result in major variations in the electrical properties of the contacts, Chip metallization is also employed to provide electrical interconnection between devices on a chip. The interconnections can all be made in a single layer, or for more complex chips, a number of layers might be employed using dielectric layers to separate metal layers and via holes through the dielectric for layer-to-layer interconnection. Chip metallization is also used to form the interconnections between the chips and the substrate carrier.

Thin film samples represent ideal samples for analysis using X-ray fluorescence in that they tend to be flat, smooth and homogeneous. However, before a sample can be characterized using XRF, several questions must be answered.

The purpose of this paper is to show how XRD and XRF can be used as complimentary tools to determine multi-layer thin film composition, both elemental and crystalline, as well as film thickness.

External X-ray total reflection occurs when collimated X-ray beams impinge on a smooth, flat surface of matter at a small glancing angle, typically a few mrad. With respect to the X-ray fluorescence technique, total reflection experiments have allowed the trace determination of solution samples using an X-ray mirror as a sample support. The grazing incidence X-ray fluorescence technique (GIF) is also suitable for near-surface element analysis of the material, because the penetration depth of X-rays is 10-1000 Å around the critical angle.

X-ray fluorescence analysis is the most suitable method, for the characterization of the thickness and the chemical composition of thin film samples. It is non-destructive, rapid, precise, and accurate for both metal and oxide samples.

The fundamental parameter method for x-ray spectrometry has been used most commonly for bulk samples, because it permits an analysis utilizing a minimum number of standards, even for samples with complicated matrices. The need for the analysis of thin film materials, which includes multi-layer films, has been increasing in recent years along with the rapid progress of high technologies. However, there have been few reports that deal with the application of fundamental parameter methods to multi-layer thin films. There may be two situations in the analysis of thin films. In routine analysis of quality control applications, they usually require precise analysis. Fortunately, it is possible to prepare well characterized standards similar to the unknowns.

The Fundamental Parameter-based calculation of x-ray fluorescence intensities for thin and multilayer samples is performed with new formulas. By the calculations it is shown that both intra- and inter-layer secondary fluorescence can cause significant enhancement. With a method based on the discussed theory, it is possible to determine the composition and layer thicknesses of multilayer samples. Analyses are discussed of samples from IC technology and magnetic recording. Furthermore, the angular dependence of intensities is calculated, in good agreement with experiments performed with a novel spectrometer.

The penetration depth of 1-12 keV electrons in most materials is less than one micron and the characteristic soft x-rays that are produced can be used to identify the elements present in the surface. Varying the energy of the incident electron beam enables the depth of analysis to be controlled.

Soft x-rays often exhibit large 'chemical effects' (changes in peak profile and peak position) which can he correlated with chemical changes. A study of such effects for each element present in the sample surface, as a function of electron-beam energy, can in some cases, permit changes in the chemical state (valency - coordination number-spin state etc.) to be determined as a function of depth.

Such analyses can be carried out either in a conventional x-ray spectrometer in which the x-ray tube has been replaced by a gas-discharge source, or in a spectrometer in which the sample is bombarded with electrons from a normal electron gun. In this paper these techniques are outlined and some applications reviewed:- the analysis of oxide layers on aluminium and steel, the analysis of aluminium-nitride layers produced by MOCVD on gallium arsenide, the analysis of silica fiims (with added boron and phosphorus oxides) on silicon and the analysis of zinc-oxide films on glass.

Two strategies are at present commonly used in studying and refining crystal structures from powder diffraction data: the total pattern refinement proposed by Rietveid (1969) and the two-step method originally proposed and applied by Will (Will et al., 1965). The latter one works by separating-the intensity determination of the individual peaks from the actual structure refinement, structure analysis or any structural calculation (tor example based on line broadening). Both methods have their merits, and their drawbacks.

The X-ray Analytical Science Group at Curtin university of Technology has been developing and evaluating Rietveld pattern-fitting for materials analysis since 1985. The results are reviewed with particular reference to preferred orientation, crystallinity and phase abundance.

Texture means the orientation distribution of the many crystallites in a polycrystalline sample with respect to a reference system on the sample, for example the rolling direction in steel. Texture has to be distinguished from preferred orientation observed in laboratory-made powder samples. Preferred orientation is just a nuissance in the experiment and must be corrected in the ensuing analysis, for example by the formula given by March and published by Dollase Preferred orientation we find commonly in samples containing plate-like crystal flakes. This is again to be distinguished from a non-random particle distribution in the powder samples prepared for diffraction experiments. This effect is always present, also for example in NBS silicon, even if only to a. very small degree (see for example Will et. al). It must and can easily be corrected for in the final least-squares calculation.

Most commercially available, automated powder diffractometers include software packages for the determination of d-values from experimentally recorded digitized patterns. While many of these patterns offer great flexibility to the user, indications from a recent Round-Robin Study [1] are that many users are confused as to the correct use of such parameters as choice of step size and counting time, the degree of data smoothing, peak-hunting parameters, setting of background level, and the consequences of background subtraction and α2 stripping. This paper will reviews these various factors and give some guidelines as to the establishment of optimum conditions.

A precise and practical method for the determination of d-values and lattice parameters from digital diffraction data is described. Systematic errors are corrected mathematically during a d-spacing / lattice-parameter least-Squares refincment process making it unnecessary to use internal standards. X-ray and synchrotron diffraction data of an ICDD alumina plate obtained with a wide variety of experimental conditions and analysis parameters were used to study the precision in the derivation of d-values and the accuracy in the determination of lattice parameters. Results showed that the precision in determining d-values was high with |Δd/d|avg ranging from 2x105 to 4x10-5. Using the results obtained from the high precision XRD analysis as a reference standard, the accuracy in the lattice parameter determinations from the synchrotron diffraction data reached the l-2x10-6] range. Lattice parameters, with an accuracy in the high 10-5 range, were also obtained using parameters commonly used in a routine XRD analysis such as a wide RS (0.11°) for high intensity, peaks only in the front reflection region, no Kα2 stripping, and a Single 2θo parameter for systematic error corrections.

Given a limited amount of time for data collection, what parameters do you select to generate the highest quality x-ray diffraction pattern from an automated diffractometer? This paper addresses the major topic of diffractometer step size or its equivalent, chopper size, for instruments running in the continuous scanning mode. In general, step size and chopper size will be interchanged freely. A minor topic intertwined into the discussion will be the receiver slit width.

The use of high-intensity, 8Kw, x-ray sources (Rigaku rotating-anode generator and wide - angle goniometer for this study) provides both opportunities and challenges. With high - intensity x-ray sources, detection limits can be lowered significantly while still offering count times of practical duration. On the other hand, the availability of high intensity x-ray sources puts greater demands on information extraction procedures and on the mechanical preciseness of sample containment and support. In particular we addressed the use of a cylindrical aluminum sample cell with a 0.010’’ polycrystalline (cold rolled) beryllium window electron –beam welded to an aluminum frame. See Figure 1. This cell permitted analysis of various air-sensitive specimens. The sample was pressed against the back of the beryllium window by a spring-loaded backing plate.

The residual stress left on the fracture surface is one of the important parameters in X-ray fractography. It has been used to analyze fracture mechanisms in fracture toughness and fatigue tests especially of iron and steels.

In the present paper, X-ray fractography was applied to the brittle fracture surface of a silicon nitride ceramics. The first part deals with the determination of the stress constant for diffraction from Si3N4(411) plane by Cr-Kα radiation. The second part describes the effect of the notch-tip radius on the fracture toughness value. In the last part, the plastic zone depth was determined from the residual stress destribution beneath the fracture surface.

X-ray fractography is a new method utilizing the X-ray diffraction technique to observe the fracture surface for the analysis of the micromechanisms and mechanics of fracture. The X-ray residual stress has been confirmed to be a particularly useful parameter when studying the fracture surfaces of high strength steels. The method has been applied to the fracture surface of fracture toughness and fatigue specimens.

X-ray stress analysis is widely used in the measurement of residual stress or stress under static loading. If it is possible to measure actual stress at any applied stress level during cyclic loading by using x-rays, it will be of much help in investigating dynamical fatigue behavior such as crack closure and change of residual stress distribution.