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Analysis of Modified Williamson-Hall Plots on GaN Layers

This article has been downloaded from IOPscience. Please scroll down to see the full text article. 2011 Chinese Phys. Lett. 28 016101 (http://iopscience.iop.org/0256-307X/28/1/016101) View the table of contents for this issue, or go to the journal homepage for more

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CHIN. PHYS. LETT. Vol. 28, No. 1 (2011) 016101

Analysis of Modified Williamson-Hall Plots on GaN Layers

LIU Jian-Qi()1,2,3 , QIU Yong-Xin()1 , WANG Jian-Feng()1 , XU Ke()1** , YANG Hui()1

1

Platform for Characterization & Test, Suzhou Institute of Nano-Tech and Nano-Bionics, Chinese Academy of Sciences, Suzhou 215125 2 Institute of Semiconductors, Chinese Academy of Sciences, Beijing 100083 3 Graduated University of Chinese Academy of Sciences, Beijing 100049

(Received 12 May 2010)

WilliamsonHall (W-H) analysis is often used to separate the lateral coherence length (LCL) broadening and dislocation broadening on the -scan with a Lorentzian distribution. However, besides the LCL broadening and dislocation broadening, curvature also can broaden the -scan peak. Usually, the -scan can be described by a Pseudo-Voigt (P-V) function more precisely than a Lorentzian function. Based on the P-V fit peak profile, we modify the W-H plots. Both LCL broadening and curvature broadening can be eliminated from (00) -scans plots simultaneously, and a reliable tilt can be obtained. This method is a good complementary for the existing method, but is more convenient. Although we focuse on GaN layers, the results are applicable to a wide range of other materials having mosaic structures.

PACS: 61. 05. Cp, 81. 05. Ea

DOI: 10.1088/0256-307X/28/1/016101 High-resolution x-ray diffraction (HRXRD) is a widely used, fast and nondestructive method to characterize the mosaic structure of GaN layers. Historically, WilliamsonHall (W-H) plots[6,7] (often used to separate the effects of different factors that contribute to x-ray -scan or 2/-scan line broadening) are widely used to obtain the tilt angle, vertical coherence length and LCL of the GaN layers. Usually, the W-H method needs to record a series of (00) scans and 2/-scans. However, wafer curvature is often a significant (00) -scan broadening besides LCL and dislocation broadenings. When the GaN layers are grown thick, they always highly curved. Therefore, W-H analysis of (00) -scan will be unreliable for curved samples as pointed by Moram et al.[8] However, it has been well known that the curvature broadening effect can be eliminated conventionally by a routine method:[9] x-ray -scan measurements are carried out with a variety of slit-width ( ) for incident x-ray beam, and then the breadths are plotted against . The value for -scan breadth without the effect of curvature is obtained from = 0 and the curvature from the slope. Diffraction peaks are broadened by factors that relate to the instrument and the sample structure. The separation (deconvolution) of all the broadening factors (mainly dislocation broadenings, LCL broadenings and curvature broadenings) is complicated based on the existing method.[7,9] First the (002), (004), and (006) -scan measurements are performed with a variety of , and the breadths are plotted against

Gallium nitride (GaN) and its alloys have attracted significant attention in recent years due to the successful development of visible and ultraviolet lightemitting-diodes (LEDs),[1] blue/violet laser diodes,[2] and high-power electronic devices.[3] However, most III-nitrides layers are generally bent, highly faulted and manifest a mosaic structure consisting of many small hexagonal grains, due to large mismatch in lattice constants and thermal expansion coefficients between III-nitrides layers and substrates such as sapphire, silicon or silicon carbide.[4] The mosaic structure of GaN layers is usually described by a columnar model with four parameters: tilt angle , twist angle, vertical coherence length and lateral coherence length (LCL) , as illustrated in Fig. 1. Although more sophisticated models describing dislocations may be applied with improving quality of GaN films,[5] the simple mosaic structure model works well in most cases.
Tilt Twist L//

Lu

Fig. 1. Columnar model for the mosaic structure of GaN layers.

* Supported by the National Natural Science Foundation of China under Grant Nos 60776003 and 10704052, and the National Basic Research Program of China under Grant No 2007CB936700 ** Email: kxu2006@sinano.ac.cn c 2011 Chinese Physical Society and IOP Publishing Ltd

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to obtain the -scan breadth without the curvature effect. Then the (00) -scan breadths without curvature effect are plotted by the use of the W-H method to obtain the dislocation broadenings. Such a method needs record many x-ray diffracted curves for one sample. An effective approach is to simulate experimental data by convoluting models for broadening factors together. In this Letter, we modified the W-H plots to eliminate LCL and dislocation broadenings together, and to obtain the exact tilt angle . Also, LCL or the radius of curvature from the GaN layers can be obtained by using the modified W-H plots.

half-maximum (FWHM) of -scan denoted by 0 , which is normally much narrower than that of the actually measured FWHM . In addition to the intrinsic width 0 , there are some other main factors which could contribute to the broadening of -scan: (a) the broadening due to x-ray beam divergence , (b) the broadening due to dislocations , and (c) the broadening due to finite LCL , (d) the broadening due to curvature of the heteroepitaxial layer, . Thus, the FWHM of the measured -scan can be expressed as[1114]
= 0 + + + + .

(1)

Beam width W

B Surface of the specimen Ds

Fig. 2. Schematic diagram of x-ray -scan measurement for a curved specimen.

The individual terms are folded using Gaussian ( = 2), PseudoVoigt (P-V) (1 < < 2), or Lorentzian ( = 1) distributions.[12,13] 0 is usually less than 10 arcsec. Here depends on the beam conditioner. For the beam conditioner with four reflections or eight reflections, it is usually less than 12 arcsec. For most III-nitrides, the dislocation density is higher than 106 cm2 , and the broadening is often larger than 100 arcsec. Therefore, Eq. (1) can be rewritten as + + , (2) and the value of , which is related to the LCL, is given by[6,15] = /(2 sin ), (3)

Four GaN samples studied in our work were grown on (0001)-oriented sapphire substrates. Samples A and B with thicknesses 0.6 m and 3.0 m were grown by metal organic chemical vapor deposition (MOCVD). Samples C and D with thicknesses 20 m and 38 m were grown by hydride vapor phase epitaxy (HVPE). A four-circle Bruker D8 Discover HRXRD (using Cu 1 radiation) equipped with a four-bounce Ge 220 monochromator and a triple-bounce analyzer was used. The instrumental broadening was approximately 12 arcsec in -scan. The chosen horizontal x-ray slit widths were 0.1 mm and 0.8 mm, the vertical slit width is kept to be 1 mm (the vertical x-ray slit width and horizontal slit width were defined to be parallel to the diffracted plan and perpendicular to the diffracted plane, respectively). The GaN (002), (004) and (006) -scans and 2/-scans were recorded in symmetric geometry. The radius of the curvature can be measured using HRXRD[8,10] with an open detector, by recording an -scan, moving the beam across the sample by a known distance in the direction of the incoming beam and then recording a second -scan. The angular offset () between the peaks in the two scans is related to the radius of curvature by = /. However this assumes a spherical wafer curvature; therefore, the distribution of curvature was estimated by measuring the -scans of (002) reflection along and vertical to 10 direction at many points 10 separated. An ideal GaN layer has an intrinsic full-width at

where is the wave length of the x-ray, is the corresponding Bragg angle. Assuming a spherical curvature, the schematic geometry of the broadening due to curvature is shown in Fig. 2. Here is equal to the -scan broadening due to curvature of the specimen . The relationship between the radius of curvature and the can be expressed by[14,16] = / = (1/) (/sin ) = /( sin ), (4) where is the width of the x-ray beam in diffraction plane, is the radius of the curvature of the sample. From Eqs. (2)(4), we can obtain ( ) (sin /) = [(1/2 ) + (/) ] + ( ) (sin /) , (5) when is very large and = 1, Eq. (5) gives a classical WilliamsonHall type analysis. From Eq. (5) we can find that when ( ) (sin /) is plotted against (sin /) for each reflection and fitted by a straight line, the fitted line slop is a direct measure of tilt angle and the intersection 0 gives the LCL (when is very large, and a small horizontal slit is used) or the radius of curvature (when the layer is highly curved with high quality). The distribution of curvature of the four samples along and vertical to 10 direction is studied. From 10 Fig. 3 (a typically sample C), the linear fit can gives

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the radius of curvature, we can deduce that the samples we investigated have a near-spherical curvature. The curvature is defined as the average along the two directions and is listed in Table 1. All the symmetrical (00) -scan profiles recorded in triple-bounce mode from our GaN layers were fitted by a function.[12] As an example it is shown in Fig. 4. The parameter in Eq. (5) can be obtained from the fit[13] and is listed in Table 1. It is suitable to use the theoretical approach developed in Eq. (5) for analysis of the measured scans.
Table 1. The detailed structure of the samples from this work. Thickness (m) 0.6 3.0 20 38 (m) 29.3 5.8 1.8 1.1 1.4 1.4 2.0 2.0 (arcsec) 570 205 118 106 (nm) 615 1385 (m)

ings are listed in Table 1. Also, an approximate radius of curvature can be obtained from the intersection 0 (omitting the LCL effects), which is also listed in Table 1. The obtained is almost the same as the previous measured , which indicates that the modified W-H plots and omitting the effects are suitable for our samples.

Measured Pseudo-Voigt fit

Sample Sample Sample Sample

A B C D

1.9 1.1

Intensity

-0.15 -0.10 -0.05 0.00

18.0 17.6

Angle (deg)

0.05

0.10

0.15

Sample C Vertical to <10 1 0> Along <10 1 0>

Fig. 4. Measured GaN (006) -scan diffraction profile fitted with a function.

=1.70 m

(deg)

(10

16.8 16.4 -20 -10

-3

=1.81 m

nm)

17.2

(a)

2 1

Sample A Sample B =1.4

Position (mm)

10

20
-

sin

/ )

nm)

Fig. 3. The peak position of (002) reflection vs the site on the wafer. We define the center of the wafer as 0 point.

2 32 28 24 20 16 12 8 0 5
(b)

10

12

For samples A and B, a small horizontal slit 0.1 mm can almost eliminate the broadening due to curvature ( is estimated from Eq. (4)). The characteristics of ( ) (sin /) plotted against (sin /) are shown in Fig. 5(a). The LCL and tilt are obtained from the intersection 0 and the slop, and is listed in Table 1. We can see that, when the thickness of the GaN layer reaches several microns, the LCL reaches several microns too, which can make the LCL broadening less important. For the thicker samples C and D, they are highly curved and have low dislocation density (about 108 /cm2 ). Their LCL must be larger than sample B. It is considered that the LCL effect is negligible, which is also consistent with former studies.[12,13] However, the curvature broadening remains large even a small horizontal slit is used.[17] The curvature broadening effects can be eliminated by Eq. (5). A larger horizontal slit 0.8 mm is used to minimize the testing time without losing resolution. Figure 5(b) shows the modified W-H plots of the samples C and D, the obtained net dislocation broaden-

(10

-6

Sample C Sample D =2

sin

/ )

10

15
(sin

20
/ )

25
(nm)
-

30

35

Fig. 5. Modified Williamson-Hall plots of -scan peak width for the (00) series of reflections from different thicknesses and dislocation densities GaN layers, assuming a Pseudo-Voigt line shapes. (a) Samples A and B, (b) samples C and D (see the details in Table 1).

In fact, to separate the broadening caused by LCL, curvature and dislocation are complicated by use of the existing methods[7,9] for many of the large mismatch layers. However, the modified W-H plots can separate the broadening caused by dislocation and the other two parts simultaneously. Usually, the dislo-

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cation broadening is the most important parameter to characterize the crystal quality. The dislocation broadening obtained from the modified W-H plots is reliable and has nothing with the measurement condition. However, the accuracy of the obtained parameters LCL or radius of curvature obtained from the modified W-H plots severely depends on the sample and measurement condition. Since the line width in 2/-scan does not contain the effect of curvature in principle. We employ the usual W-H plots to 2/-scans for estimation of vertical coherence length in the samples. The estimated contribution to the broadening of 2/-scans due to the vertical coherence length is too small (close to the precision of measurements of curve broadening) and could not lead to reliable results for samples B, C and D. In conclusion, modified W-H plots for the accurate and convenient measurement of the mosaic structure parameters have been described. In order to exactly measure of tilt angle of the GaN layers by HRXRD, it is necessary to eliminate the LCL broadening and curvature broadening from the -scan. The modified W-H plots can be used to eliminate LCL and curvature broadening together. The LCL or radius of curvature can also be obtained from the modified W-H plots of the samples. This method is a good complementary for the existing method, and is more convenient. Although this study focuses on GaN layers, the results are applicable to a wide range of other materials having mosaic structures, which include but is not limited

to III-nitrides, ZnO and ZnSe.

References
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