International
Tables for
Crystallography
Volume H
Powder diffraction
Edited by C. J. Gilmore, J. A. Kaduk and H. Schenk

International Tables for Crystallography (2018). Vol. H, ch. 2.5, p. 145

Section 2.5.4.4.1. Crystallinity

B. B. Hea*

aBruker AXS Inc., 5465 E. Cheryl Parkway, Madison, WI 53711, USA
Correspondence e-mail: bob.he@bruker.com

2.5.4.4.1. Crystallinity

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The crystallinity of a material influences many of its characteristics, including mechanical strength, opacity and thermal properties. Crystallinity measurement provides valuable information for both materials research and quality control in materials processing. The diffraction pattern from a material containing both amorphous and crystalline solids has a broad feature from the amorphous phase and sharp peaks from the crystalline phase. The weight percentage of the crystalline phases in a material containing both crystalline and amorphous phases can be determined by X-ray diffraction (Chung & Scott, 1973[link]; Alexander, 1985[link]; Murthy & Barton, 2000[link]; Kasai & Kakudo, 2005[link]). Assuming that the X-ray scattering intensity from each phase in such a material is proportional to its weight percentage, and that the scattering intensities from all phases can be measured within a given 2θ range, the per cent crystallinity is given by[{x_{\rm pc}} = 100\% {{{I_{\rm crystal}}} \over {{I_{\rm crystal}} + {I_{\rm amorphous}}}},\eqno(2.5.90)]where xpc is the per cent crystallinity, Icrystal is the integrated intensity of all crystalline peaks and Iamorphous is the integrated intensity of the amorphous scattering. The accuracy of the measured per cent crystallinity depends on the integrated diffraction profile. Since most crystalline samples have a preferred orientation, it is very difficult to obtain a consistent measurement of crystallinity with a conventional diffractometer. Fig. 2.5.28[link] 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. Fig. 2.5.28[link](a) shows a diffraction profile integrated from a horizontal region analogous to a profile collected with a conventional diffractometer. Only one peak from the crystalline phase can be observed in the profile. It is also possible that a different peak or no peak is measured if the sample is loaded in other orientations. Fig. 2.5.28[link](b) is the diffraction profile integrated from the region covering all peaks from the crystalline phase over almost all azimuthal angles. A total of four peaks from the crystalline phase are observed. This shows that a 2D-XRD system can measure per cent crystallinity more accurately and with more consistent results (Pople et al., 1997[link]; Bruker, 2000[link]) than a conventional system.

[Figure 2.5.28]

Figure 2.5.28 | top | pdf |

2D diffraction pattern from an oriented polycrystalline polymer sample. (a) Diffraction profile integrated from a horizontal region analogous to a profile collected with point detector. (b) Diffraction profile integrated from all parts of the 2D frame.

References

Alexander, L. E. (1985). X-ray Diffraction Methods in Polymer Science. Malabar: Krieger Publishing Company.Google Scholar
Bruker (2000). Percent crystallinity in polymer. Bruker AXS Lab Report No. L86-E00005.Google Scholar
Chung, F. H. & Scott, R. W. (1973). A new approach to the determination of crystallinity of polymers by X-ray diffraction. J. Appl. Cryst. 6, 225–230.Google Scholar
Kasai, N. & Kakudo, M. (2005). X-ray Diffraction by Macromolecules, pp. 393–417. Tokyo: Kodansha/Springer.Google Scholar
Murthy, N. S. & Barton, R. Jr (2000). Polymer industry. Industrial Applications of X-ray Diffraction, edited by F. H. Chung & D. K. Smith, pp. 495–509. New York: Marcel Dekker.Google Scholar
Pople, J. A., Keates, P. A. & Mitchell, G. R. (1997). A two-dimensional X-ray scattering system for in-situ time-resolving studies of polymer structures subjected to controlled deformations. J. Synchrotron Rad. 4, 267–278.Google Scholar








































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