Preview

Industrial laboratory. Diagnostics of materials

Advanced search

Study of the structure of fibrous carbon materials using X-ray diffractometry

https://doi.org/10.26896/1028-6861-2019-85-11-31-36

Abstract

New possibilities for diagnosing the structure of carbon materials by X-ray diffraction analysis are described. The studies were performed on an X-ray diffractometer D8 ADVANCE (filtered CuKα radiation) using carbon fibers (CF) differed in the mode of heat treatment (~2300 to ~3000°C). It is shown that when studying the structure of fibrous carbon materials characterized by a large depth of X-rays penetration, it is necessary to limit the thickness of the object under study to ~0.1 mm to provide the self-focusing condition for the entire sample volume engaged in formation of the diffracted beam. The material of high modulus carbon fibers can be heterogeneous and contain coherent scattering regions wherein the crystal structure parameters are somewhat different and experimentally observed diffraction peaks 002, 004, and 006 become asymmetric and are not described by the Gauss, Lorentz, or Voigt functions. Thus, the standard method used for determination of the average value of the interplanar spacing and the size of coherent scattering regions does provide reliable information on the real structure of the material. The profile of the asymmetric diffraction peak 002 was analyzed using the Origin program thus providing information about fine (heterogeneous) structure of the carbon fiber material which largely determines the physicomechanical properties. The data on 002 diffraction peak profiles of carbon fibers before and after removal of the CuKα2 component are presented. The data on decomposition of the experimentally observed asymmetric 002 diffraction peaks into symmetric peaks described by the Gaussian, Lorentz, and Voigt functions are compared. The most preferable is the decomposition into the components described by the Gaussian or Voigt functions.

About the Authors

V. A. Tyumentsev
Chelyabinsk State University
Russian Federation

Vasiliy A. Tyumentsev

Ul. Bratyev Kashirinykh 129, Chelyabinsk, 454001



A. G. Fazlitdinova
Chelyabinsk State University
Russian Federation

Alfiya G. Fazlitdinova

Ul. Bratyev Kashirinykh 129, Chelyabinsk, 454001



References

1. Zhua C. Zh., Yua X. L., Liua X. F., et al. 2D saxs/waxd analysis of PAN carbon fiber microstructure in organic/inorganic transformation / Chinese Journal of Polymer Science. 2013. Vol. 31. N 5. P. 823 – 832.

2. Rahaman M., Ismail A., Mustafa A. A review of Heat Treatment on Polyacrylonitrile Fiber / Polymer Degradation and Stability. 2007. Vol. 92. P. 1421 – 1432.

3. Naraghi M., Chawla S. Carbonized Micro- and Nanostructures: Can Downsizing Really Help? / Materials. 2014. N 7. P. 3820 – 3833.

4. Wang B., Xiao Sh., Cao W., et al. Evolution of Aggregation Structure of Polyacrylonitrile Fibers in the Cyclization Reaction / Journal of Applied Polymer Science. 2012. Vol. 124. P. 3413 – 3418.

5. Liu J., Xiao S., Shen Z., et al. Study on the oxidative stabilization of polyacrylonitrile fibers by microwave heating / Polymer Degradation and Stability. 2018. Vol. 150. P. 86 – 91.

6. Yang J., Liu Y., Liu J., et al. Radial and Continuous Preparation of Polyacrylonitrile-Based Carbon Fibers with Electron-Beam Irradiation Pretreatment / Materials. 2018. Vol. 11. N 8. P. 1270 – 1280.

7. Zhao W., Lu Y., Zhou L., et al. Effects on the oriented structure and mechanical properties of carbon fibers by pre-irradiating polyacrylonitrile fibers with y ray / J. Mater. Sci. 2016. Vol. 51. P. 7073 – 7084.

8. Fazlitdinova A. G., Tuymentsev V. A., Podkopaev S. A., Shveikin G. P. Changes of polyacrylonitrile fiber during thermal stabilization / J. Mater. Sci. 2010. Vol. 45. P. 3998 – 4005.

9. Ozbek S., Isaac D. Strain-induced density changes in PAN-based carbon fibres / Carbon. 2000. Vol. 38. P. 2007 – 2016.

10. Liu F., Wang H., Xue L., et al. Effect of microstructure on the mechanical properties of PAN-based carbon fibers during high-temperature graphitization / J. Mater. Sci. 2008. Vol. 43. N 12. P. 4316 – 4322.

11. Li D., Wang H., Wang X. Effect of microstructure on the modulus of PAN-based carbon fibers during temperature treatment and hot stretching graphitization / J. Mater. Sci. 2007. Vol. 42. P. 4642 – 4649.

12. Tyumentsev V. A., Fazlitdinova A. G. The relationship of production modes and the fine structure of carbon fiber / JTF. 2016. Vol. 86. Issue 3. P. 62 – 69.

13. Bukalov S. S., Leytes L. A., Goloveshkin A. S., et al. The research of carbon fiber structure obtained by high-temperature thermomechanical treatment of polyacrylonitrile filament using Raman scattering spectroscopy and X-ray diffraction / Izv. RAN. Ser. Khim. 2018. N 6. P. 1002 – 1009 [in Russian].

14. Zhu H., Li X., Han F., et al. The effect of pitch-based carbon fiber microstructure and composition on the formation and growth of SiC whiskers via reaction of such fibers with silicon sources / Carbon. 2016. Vol. 99. P. 174 – 185.

15. Cao J., Zhao W., Gao S. Properties and Structure of In Situ Transformed PAN-Based Carbon Fibers / Materials. 2018. Vol. 11. N 6. P. 1017 – 1026.

16. Lee S., Kang D., Lee S., Roh J. X-ray diffraction analysis of the effect of ball milling time on crystallinity of milled polyacrylonitrile-based carbon fibers / Carbon letters. 2018. Vol. 26. P. 11 – 17.

17. Lachter J., Bragg R. Interstitials in graphite and disordered carbons / Phys. Rev. B. 1986. Vol. 33. N 12. P. 8903 – 8905.

18. Tadjani M., Lechter J., Kabret T., Bragg R. Structural disorder induced in graphite by grinding / Carbon. 1986. Vol. 24. N 4. P. 447 – 449.

19. Aladekomo J., Bragg R. Structural transformations induced in graphite by grinding: Analyusis of 002 X-ray diffraction line profiles / Carbon. 1990. Vol. 28. N 6. P. 897 – 906.

20. Kawamura K., Bragg R. Graphitization of pitch coke: changes in mean interlayer spacing, strain and weight / Carbon. 1986. Vol. 24. N 3. P. 301 – 309.


Review

For citations:


Tyumentsev V.A., Fazlitdinova A.G. Study of the structure of fibrous carbon materials using X-ray diffractometry. Industrial laboratory. Diagnostics of materials. 2019;85(11):31-36. (In Russ.) https://doi.org/10.26896/1028-6861-2019-85-11-31-36

Views: 772


ISSN 1028-6861 (Print)
ISSN 2588-0187 (Online)