COMPARISON BETWEEN CONVENTIONAL AND TWO-DIMENSIONAL XRD

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1 Copyright JCPDS - International Centre for Diffraction Data 2003, Advances in X-ray Analysis, Volume COMPARISON BETWEEN CONVENTIONAL AND TWO-DIMENSIONAL XRD Bob B. He, Uwe Preckwinkel, and Kingsley L. Smith Bruker Advanced X-ray Solutions Madison, Wisconsin ABSTRACT A comparison between the conventional Bragg-Brentano diffractometer and the two-dimensional (2D) diffractometer is made in terms of diffraction geometry, diffraction pattern, and various applications. A two-dimensional XRD system for combinatorial screening in transmission mode is introduced. IINTRODUCTION A two-dimensional X-ray diffraction (XRD 2 ) system has both the capability of acquiring diffraction patterns in 2D space simultaneously, and analyzing the 2D diffraction data accordingly [1-3]. In recent years, usage of two-dimensional (2D) detectors has dramatically increased due to the advances in detector technology, point beam X-ray optics, and computing power. The integrated data gives better intensity and statistics for phase identification and quantitative analysis, especially for those samples with texture, large grain size, or small quantity. 2D detectors can collect diffraction data in a large 2θ range simultaneously without sample or detector movement. This is extremely important for high-throughput diffraction screening [4]. Figure 1 is a comparison between the conventional diffractometer and the two-dimensional diffractometer. The diffraction data collection in the conventional diffractometer is confined within a plane, here referred to as diffractometer plane. With a 2D detector, the measurable diffraction is no longer limited in the diffractometer plane. Instead, the whole or a large portion of the diffraction rings (as called Debye ring) can be measured simultaneously. Figure 1. Comparison of the conventional XRD and the two-dimensional XRD.

2 This document was presented at the Denver X-ray Conference (DXC) on Applications of X-ray Analysis. Sponsored by the International Centre for Diffraction Data (ICDD). This document is provided by ICDD in cooperation with the authors and presenters of the DXC for the express purpose of educating the scientific community. All copyrights for the document are retained by ICDD. Usage is restricted for the purposes of education and scientific research. DXC Website ICDD Website -

3 Copyright JCPDS - International Centre for Diffraction Data 2003, Advances in X-ray Analysis, Volume 46. The conventional diffraction pattern, collected with either a scanning point detector or a linear PSD, is a plot of X-ray scattering intensity at different 2θ angles. Figure 2 shows the conventional diffraction pattern of corundum powder. Figure 2 shows the diffraction pattern collected with a 2D detector from the same corundum sample. The 2D diffraction pattern contains far more information then the conventional diffraction pattern for applications, such as: Phase ID; Percent Crystallinity; Particle Size and Shape; Texture; and Stress [5]. Corundum Powder Diffraction Intensity Two Theta Figure 2. The diffraction pattern of corundum powder: the conventional diffraction pattern; the two-dimensional diffraction pattern. LARGE GRAIN SIZE AND TEXTURE Unlike the conventional diffraction profile, the effects of large grain size and texture can be observed directly from 2D diffraction patterns. Figure 3 shows an example. The large grain in a γ-tial sample gives a spotty diffraction ring, while a textured γ-tial sample shows the intensity variation. Reliable phase ID can be obtained from both samples by integration. Figure 3. 2D diffraction patterns from γ-tial alloys: large grain size; texture. 38

4 Copyright JCPDS - International Centre for Diffraction Data 2003, Advances in X-ray Analysis, Volume PERCENT CRYSTALLINITY The accuracy of measured percent crystallinity is dependent on the integrated diffraction profile. Since most crystallinity samples have preferred orientation, it is very difficult to have a consistent crystallinity measurement with a conventional diffractometer. Figure 4 shows a 2D diffraction frame collected from an oriented polycrystalline sample. The diffraction is in transmission mode with the X-ray beam perpendicular to the plate sample surface. Figure 4 shows a diffraction profile integrated from a horizontal region analogous to a profile collected with the conventional diffractometer. Only one crystalline peak can be observed from the profile. It means that the diffraction profile would look like the one in Figure 4 had a conventional diffractometer been used for the data collection in the same sample orientation. It is also possible that a different peak or no peak is measured if the sample is loaded in another orientation. Figure 4 is the diffraction profile integrated from all parts of the 2D frame. A total of four crystalline peaks are observed. Apparently, the percent crystallinity measured with the conventional diffractometer is not consistent if the preferred orientation is not considered. While the sample orientation has no effect on the full circle integrated diffraction profile from a 2D frame, an XRD 2 system can measure percent crystallinity more accurately with consistent results. Figure 4. 2D diffraction pattern from an oriented polycrystalline sample. Diffraction profile integrated from a horizontal region analogous to a profile collected with point detector. Diffraction profile integrated from all parts of the 2D frame.

5 Copyright JCPDS - International Centre for Diffraction Data 2003, Advances in X-ray Analysis, Volume INSTRUMENT BROADENING Conventional diffractometers use the Bragg-Brentano parafocusing geometry [6] as is show in Figure 5. A divergent beam from the X-ray tube passes first through the divergent slit, then hits the sample surface with an incident angle θ. The incident X-rays spread over the sample surface with various incident angles in the vicinity of θ. The area of irradiated region depends on the incident angle θ and beam divergence. The diffracted rays from the irradiated area leave the sample at an angle 2θ from the corresponding incident rays, pass through the anti-scatter slit, and focus at the detector slit. The instrument broadening can be controlled by both slit size and scanning step. Figure 5. A conventional diffractometer in Bragg-Brentano geometry In an XRD 2 system, the diffracted X-rays are measured simultaneously in a two-dimensional range so no slit or scanning step can be used to control the instrument broadening. The beamspread over the sample surface can not be focused back to the detector. Figure 6 shows geometry of two-dimensional diffraction in reflection mode and transmission mode. Defocusing effect is observed with low incident angle over a flat sample surface in reflection mode diffraction. In reflection mode, the diffracted beam in low 2θ angle is narrower than the diffracted beam in high 2θ angle. In transmission mode with the incident beam perpendicular to the sample surface, no such a defocusing effect is observed. Figure 6. Geometry of XRD 2 : reflection mode; transmission mode. If one looks at the cross section on the diffractometer plane and forward diffraction (2θ<90 ) only, the defocusing effect with reflection mode diffraction can be expressed as:

6 Copyright JCPDS - International Centre for Diffraction Data 2003, Advances in X-ray Analysis, Volume B b = sin( 2θ ω) (1) sinω where ω is the incident angle, b is the incident beam size and B is diffracted beam size. The defocusing with transmission mode with a perpendicular incident beam can be given as: B t = cos2θ + sin2θ (2) b b where t is the sample thickness. If the sample thickness t is negligible compared to the incident beam size b, we have: B b = cos2θ 1 (3) There should be no defocusing effect at all. Figure 7 is a comparison between reflection mode and transmission mode diffraction with data frames collected from corundum powder. With 5 incident angle, the reflection pattern shows severe peak broadening compared with no defocusing in transmission mode pattern. Figure 7. Diffraction pattern from corundum: reflection mode diffraction 5 incident angle, transmission mode diffraction with perpendicular incident beam. TWO-DIMENSIONAL XRD FOR COMBINATORIAL SCREENING A two-dimensional diffraction system designed for XRD combinatorial screening in reflection mode has been introduced previously [4]. In many combinatorial screening applications, such as polymorphism study in pharmaceutical chemistry and catalysis development in the oil industry, a typical 2θ measuring range is from 2 to 60. It is necessary to run the combinatorial XRD screening in transmission mode in order to avoid the defocusing effect. A two-dimensional diffraction system is designed for XRD screening in transmission mode for various applications, including screening of material libraries for combinatorial chemistry. As is shown in Figure 8, the system is built on a vertical two-circle goniometer. An offset mounted XYZ translation stage yields space for X-ray source, optics, and X-ray detector, while it provides translations in X, Y and Z directions for material library scanning and sample alignment. A laser/video sample alignment system is mounted on the outer circle of the goniometer so that it can be driven away

7 Copyright JCPDS - International Centre for Diffraction Data 2003, Advances in X-ray Analysis, Volume after alignment. An optional motorized beamstop has two positions, retracted position for loading, unloading and aligning sample, and extended position during diffraction and scattering measurement. In the transmission mode X-ray diffraction measurement, the incident beam is typically perpendicular to the sample so the irradiated area on the specimen is limited to a size comparable to the X-ray beam size, allowing the X-ray beam concentrated to the intended measuring area. In combinatorial screening applications, sample cells are located close to each other. Therefore, The transmission mode diffraction can also avoid cross contamination between adjacent samples. Figure 8. Transmission diffraction system for combinatorial screening. CONCLUSION The two-dimensional diffraction provides far more information than the conventional onedimensional diffraction. However, in order to utilize the extra information gained from 2D diffraction, distinct features of two-dimensional diffraction must be taken into account. REFERENCES [1] Philip R. Rudolf and Brian G. Landes, Two-dimensional X-ray Diffraction and Scattering of Microcrystalline and Polymeric Materials, Spectroscopy, 9(6), pp 22-33, July/August [2] S. N. Sulyanov, A. N. Popov and D. M. Kheiker, Using a Two-dimensional Detector for X- ray Powder Diffractometry, J. Appl. Cryst. 27, pp , [3] B. B. He, U. Preckwinkel and K. L. Smith, Fundamentals of Two-dimensional X-ray Diffraction (XRD2), Advances in X-ray Analysis, Vol. 43, Proceedings of the 48th Annual Denver X-ray Conference, Steamboat Springs, Colorado, USA, [4] B. B. He, et al, XRD Rapid Screening System for Combinatorial Chemistry, Advances in X- ray Analysis, Vol. 44, Proceedings of the 49th Annual Denver X-ray Conference, Denver, Colorado, USA, [5] B. B. He, Introduction to 2D XRD, Bruker AXS Document # M86-E [6] Ron Jenkins and Robert L. Snyder, Introduction to X-ray Powder Diffractometry, John Wiley & Sons, New York, 1996.

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