X-RAY DIFFRACTION

Cammille Louise P. Carinan
X-ray diffraction (XRD) is a technique that uses X-ray beams as a monochromatic source to determine the properties of an element or compound; it can determine the average spacing between atoms and the orientation, size, and structure of its crystals [1]. It utilizes the dual wave-particle property of the X-ray to obtain these data [2]. XRD is also used in characterizing semiconductors; properties such as lattice parameters, epitaxial layer thickness and mole fraction can be determined [1]. In this paper, the unknown parameters of an A/B/A/B superlattice is investigated using XRD. The sample used is an AlxGaAs1-x/GaAs heterostructure with N=40 that is grown using Molecular Beam Epitaxy. Its layer thickness and mole fraction are unknown.

Mole Fraction
Some properties of a semiconductor alloy is dependent to its mole fraction, such as its bandgap and its lattice parameters [1]. In connection with the latter, there is an empirical law which states that the mole fraction and the lattice parameters of the alloy has an approximate linear relationship, and that law is known as the Vegard’s law [3]. Vegard’s law is described by the equation 𝑎 𝐴𝐵 (𝑥) = 𝑎 𝐴 𝑥 + 𝑎𝐵 (1 − 𝑥) where x is the mole fraction of an alloy AxB1-x, aA, aB, and aAB are the lattice constants of the metal A, metal B and the alloy, respectively [4]. Relating this rule to the XRD scan, it is seen that the mole fraction can be obtained using the relationship 𝑥 = ∆𝜃 ∆𝜃0

where Δθ is the angle difference of the resulting peaks of the metals that comprises the ion. According to Chang, et.al, the mole fraction of Al in the ternary compound AlxGaAs1-x is given by 𝑥𝐴𝑙 = where the ∆𝜃0 is the Vegard’s constant of GaAs [5]. ∆𝜃 375

Figure 1. The XRD mole fraction scan of the sample

The sample was subject in an XRD scan from -400 to 200 arcseconds with increments of 0.715 arcseconds. The resulting plot is shown in Figure 1. It is seen that there are two distinct peaks; the large peak with a relative intensity of 37469.6 and a smaller peak with a relative intensity of 8496.09. The plot is centered at the large peak for it to be in the zeroth order, which is at 0°, since this peak denotes the GaAs substrate and layers. The small peak, on the other hand, is located at 96.001°. The angle difference ∆𝜃 is then equal to 96.001°. Using this in Equation 3, the mole fraction of Al is obtained to be 0.256. This mole fraction will be used for the next scan.

Period Thickness
Errors are inevitable in growing semiconductors – the nominal layer thickness of the superlattices and multiple quantum wells is usually different from the grown layers. One way to measure this is by using XRD to measure the period thickness. According to Mr. Abat, the period thickness can be obtained from the XRD plots using the equation Λ= |𝑛𝑖 − 𝑛𝑗 |𝜆 |𝑠𝑖𝑛𝜃𝑖 − 𝑠𝑖𝑛𝜃𝑗 |

where λ is the X-ray wavelength, which is equal to 1.5406Å, 𝑛𝑖 and 𝑛𝑗 are the orders of the central peak and the satellite peak and 𝜃𝑖 and 𝜃𝑗 are its peak locations [6]. A rocking curve scan of the sample from 29.6° to 33.6° was made, and this is shown in Figure 2. Logarithmic scale was applied to the y-axis to discern the intensities from other orders since the central peak is very distinct. It was observed that the central peak, which is located at 31.5778°, have

two protruding peaks instead of one, and this is caused by the GaAs substrate and layers. The plot was then translated in order for the central peak is at 0°. Other peaks can also be distinguished: two n=1 peaks at 30.9517° (-0.6251°) and 32.2176° (0.6402°) and one n=2 peak at 32.7613° (1.1835°). The periodic thickness of the sample can be found using Equation 4, and the values obtained per order were tabulated in Table 1. The average periodic thickness of the sample was found to be 142.7572 Å.

Figure 2. The XRD rocking curve scan of the sample

Table 1. The computed period thickness of the sample

n = 1 at -0.6251° n = 1 at 0.6402° n = 2 at 1.1835° average

period thickness (Å) 141.212 137.8815 149.1781 142.7572

Now that the period thickness was obtained, it would be better if the individual layer thickness could be also found. One method of determining their values is by fitting a simulation program to the XRD plot of the sample. The best fit of the program plot to the XRD plot is shown by Figure 3. It is observed that the peaks of the simulation plot coincide the XRD plot perfectly, except for order n = 2. To achieve this fit, layer A (AlGaAs) thickness was found to be 122Å while layer B (GaAs) thickness is 22Å.

The period thickness yielded by the program is equal to 144Å. This deviates from the computed value by 0.8631% only. This means that the fit of the simulation program, even though the n=2 order does not overlap well, is acceptable.

References:

[1] X-Ray Diffraction <http://web.pdx.edu/~pmoeck/phy381/Topic5a-XRD.pdf> Retrieved 22 February 2013 [2] Introduction to X-Ray Powder Diffraction <http://epswww.unm.edu/xrd/xrdclass/01-XRD-Intro.pdf> Retrieved 22 February 2013 [3] De Graef, M. “Structure of Materials: An Introduction to Crystallography, Diffraction, and Symmetry.” Cambridge University Press, 2007 [4] Alloy Semiconductors < http://www.ecse.rpi.edu/~schubert/Course-Teaching-modules/A010-Alloysemiconductors.pdf> Retrieved 19 February 2013 [5] Chang, K.H., Precise determination of aluminum content in AlGaAs. Journal of Applied Physics. 1991;70(9):4877 [6] Abat, J.R.R., “Kinematical model of x-ray diffraction on multilayered superlattices.” Thesis. National Institute of Physics, University of the Philippines Diliman, 2011. Print.