Abstract
In this article, we focus on the structural peculiarities of nanosized Fe3O4 in the core-shell nanocomposites obtained by polymerization of conducting polypyrrole shell around Fe3O4 nanoparticles. The local structure of Fe atoms was determined from the Extended X-ray Absorption Fine Structure analysis using our own package computer programs. An X-ray diffraction method that is capable to determine average particle size, microstrains, as the particle size distribution of Fe3O4 nanoparticles is presented. The method is based on the Fourier analysis of a single X-ray diffraction profile using a new fitting method based on the generalized Fermi function facilities. The crystallites size obtained by X-ray diffraction spectra analysis was estimated between 3.2 and 10.3 nm. Significant changes in the first and the second Fe coordination shell in comparison with standard bulk were observed. The global and local structure of the nanosized Fe3O4 are correlated with the synthesis conditions of the core-shell polypyrrole nanocomposites.
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Abbreviations
- k :
-
Wave vector
- A j (k):
-
Amplitude function
- R i :
-
The radial distance
- N i :
-
Number of atoms
- F i (k,r,π):
-
Backscattering amplitude
- s :
-
Scattering parameter
- WF(k):
-
Apodization windows
- h :
-
Experimental X-ray line profile
- g :
-
Instrumental X-ray line profile
- f :
-
True sample function
- H(L):
-
Fourier transform of h profile
- G(L):
-
Fourier transform of g profile
- F(L):
-
Fourier transform of true sample function
- F (s)(L):
-
Fourier transform contribution about crystallite size and stocking fault probability
- \( F^{(\epsilon)} (L) \) :
-
Fourier transform contribution about microstrain of the lattice
- D eff(hkl):
-
Effective crystallite size
- \( \langle \epsilon^{2} \rangle_{hkl} \) :
-
Microstrain of the lattice
- A,a,b,c :
-
Parameters of generalized Fermi function
- ΔN :
-
Uncertainties of atom numbers
- ΔR :
-
Uncertainties of coordination shell
- ΔE 0 :
-
Uncertainties of K edge position
- FWHM :
-
Full width at half maximum of true sample function
- D Sch :
-
Crystallite size from Scherrer relation
- μ:
-
Absorption coefficient
- χ:
-
EXAFS function
- σ:
-
Root means squares
- λ:
-
Mean free path function for inelastic scattering
- Φ:
-
Radial structure function
- δh :
-
Integral width of experimental profile
- δf :
-
Integral width of true sample function
- j :
-
Coordination shell
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Acknowledgments
The authors are grateful to BSRF for the beam time, and to Drs. Hu Tiandou and Liu Tao for their technical assistance in EXAFS and XRD measurements. The author (N. A.) is also indebted to Professors Chen Hesheng, director of The Institute of High Energy Physics, and Fang Shouxian, director of The BEPC National Lab., respectively, for their hospitality during his stay. This work is the result of the Scientific Cooperation Agreement between our institutes. This work was supported by the research programmers of The Romanian Ministry of Education and Research (CEEX-MATNANTECH projects nr. 12/2005 and CNCSIS nr. 1484).
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Aldea, N., Turcu, R., Nan, A. et al. Investigation of nanostructured Fe3O4 polypyrrole core-shell composites by X-ray absorbtion spectroscopy and X-ray diffraction using synchrotron radiation. J Nanopart Res 11, 1429–1439 (2009). https://doi.org/10.1007/s11051-008-9536-3
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DOI: https://doi.org/10.1007/s11051-008-9536-3