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. 2017 Aug 29;2(8):5128-5136.
doi: 10.1021/acsomega.7b00668. eCollection 2017 Aug 31.

Insights into the Local Structure of Tb-Doped KY3F10 Nanoparticles from Synchrotron X-ray Diffraction

Rodrigo U Ichikawa  1 , Horacio M S M D Linhares  2 , Inma Peral  3   4 , Sonia L Baldochi  1 , Izilda M Ranieri  1 , Xavier Turrillas  5   6 , Luis G Martinez  1
Affiliations

Insights into the Local Structure of Tb-Doped KY3F10 Nanoparticles from Synchrotron X-ray Diffraction

Rodrigo U Ichikawa et al. ACS Omega. .

Abstract

Pure and Tb-doped nanocrystalline KY3F10 specimens were synthesized by coprecipitation, and portions of the samples underwent further heat treatment at 600 °C in a fluorinated atmosphere. Synchrotron X-ray diffraction patterns acquired at 30 keV allowed to determine both long- and short-range ordered structures by Rietveld and pair distribution function (PDF) analyses, respectively. PDF examination of the as-synthesized sample allowed to discern a slight deviation from the basic cubic building unit because the Y-F bond lengths could be explained in S.G. I4/mmm with cell parameters a = 8.1520(9) Å and c = 11.5876(29) Å, whereas Rietveld analysis could equally well fit both the cubic and tetragonal descriptions for the heat-treated specimens. Also, PDF revealed that the as-synthesized sample exhibited less structural coherence than the heat-treated one.

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Conflict of interest statement

The authors declare no competing financial interest.

Figures

Figure 1
Figure 1
Basic unit of the structure. A central Y atom linked to eight F atoms. The coordination polyhedron is a square antiprism.
Figure 2
Figure 2
Two alternative views of the basic assemblages [Y6F20]2– composed of six cubic antiprisms: (a) around an empty cube formed by eight F1 atoms and (b) around an empty cuboctahedron formed by 12 F2 atoms. Potassium atoms are omitted for clarity.
Figure 3
Figure 3
KY3F10 global structure along [1 0 0] on top and along [1 1 0] at the bottom part. The connections between the [Y6F20]2– assemblages are shown with the unit cell highlighted inside the rectangles.
Figure 4
Figure 4
Experimental (symbols) and calculated (black solid line) synchrotron powder diffraction profiles. The profiles were calculated with Rietveld refinement for the (a) as-synthesized Tb:KY3F10, (b) heat-treated Tb:KY3F10, and (c) pure KY3F10 samples. Below the profiles (gray solid line) is the difference between calculated and experimental values. The position of the Bragg peaks is given by the vertical bars at the bottom of the plots.
Figure 5
Figure 5
Experimental (symbols) and calculated (black solid line) atomic pair distribution functions G(r) of synchrotron powder diffraction data. Below the functions (gray solid line) is the difference between calculated and experimental values. PDF modeling was performed through PDFgui using the cubic structure for (a) Tb:KY3F10 as-synthesized, (b) Tb:KY3F10 heat-treated, and (c) pure KY3F10 heat-treated samples. The arrows indicate a mismatch in the first PDF peak.
Figure 6
Figure 6
Assemblage of [Y6F20]2– inside the tetragonal cell. Antiprisms with different inner yttrium atoms are colored differently: Y1, dark gray; Y2, light gray.
Figure 7
Figure 7
Experimental (symbols) and calculated (black solid line) atomic pair distribution functions G(r) of synchrotron powder diffraction data. Below the functions (gray solid line) is the difference between calculated and experimental. The PDF modeling was performed through PDFgui using the tetragonal structure for (a) Tb:KY3F10 as-synthesized, (b) Tb:KY3F10 heat-treated, and (c) pure KY3F10 heat-treated samples.
Figure 8
Figure 8
Experimental (symbols) and calculated (black solid line) atomic pair distribution functions G(r) of synchrotron powder diffraction data fitted up to 100 Å. Below the functions (gray solid line) is the difference between calculated and experimental values. The PDF modeling was performed through PDFgui using the tetragonal structure for (a) Tb:KY3F10 as-synthesized, (b) Tb:KY3F10 heat-treated, (c) pure KY3F10 heat-treated samples.
Figure 9
Figure 9
Distortion ratio evolution with fitting r range of the PDF for the three samples.
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References

    1. Kui H. W.; Lo D.; Tsang Y. C.; Khaidukov N. M.; Makhov V. N. Thermoluminescence properties of double potassium yttrium fluorides singly doped with Ce3+, Tb3+, Dy3+ and Tm3+ in response to α and β irradiation. J. Lumin. 2006, 117, 29.10.1016/j.jlumin.2005.03.012. - DOI
    1. Zhu L.; Cao X. Q.; Yang D. W. Facile Synthesis of Monodisperse KY3F10 Nanospheres. Adv. Mater. Res. 2011, 233–235, 2736.10.4028/www.scientific.net/AMR.233-235.2736. - DOI
    1. Cao C.; Yang H. K.; Moon B. K.; Choi B. C.; Jeong J. H.; Kim K. H. Hydrothermal synthesis, phase evolution, and optical properties of Eu3+-doped KF–YF3 system materials. J. Mater. Res. 2012, 27, 2988.10.1557/jmr.2012.331. - DOI
    1. Linhares H. M. S. M. D.Síntese de nanocristais de KY3F10 pelo método de co-precipitação visando aplicações ópticas. Ph.D. Thesis, Universidade de São Paulo, São Paulo, Brazil, 2014.
    1. Gomes L.; Linhares H. M. S. M. D.; Ichikawa R. U.; Martinez L. G.; Ranieri I. M. Luminescence properties of Yb:Nd:Tm:KY3F10 nanophosphor and thermal treatment effects. J. Lumin. 2015, 157, 285.10.1016/j.jlumin.2014.08.048. - DOI