XIV
h
International Conference on Molecular Spectroscopy, Białka Tatrzańska 2017
168
T1: P–35
Synthesis and spectral characterization of TiO
2
- and Fe
2
O
3
-halloysite
nanocomposites
Paweł Rogala
1
, Beata Szczepanik
1,2
, Piotr M. Słomkiewicz
1,2
, Dariusz Banaś
3,4
,
Aldona Kubala-Kukuś
3,4
, Ilona Stabrawa
3,4
1
Institute of Chemistry, Jan Kochanowski University, Świętokrzyska 15G, 25-406 Kielce, Poland
2
The Structural Research Laboratory, Jan Kochanowski University, Świętokrzyska 15G, 25-406
Kielce, Poland
3
Institute of Physics, Jan Kochanowski University, Świętokrzyska 15, 25-406 Kielce, Poland
4
Holycross Cancer Center, Artwińskiego 3, 25-734 Kielce, Poland
Halloysite is a 1:1 layered mineral with one silica tetrahedron sheet and one alumina
octahedron sheet [1]. The tubular nanostructure, chemical stability, high specific surface area
and porosity, and large adsorption capacity make it attractive for technological applications [2].
The structure of halloysite has been modified in different way to obtain new adsorbents,
photocatalysts or photocatalyst supports. For example, TiO
2
-clay nanocomposites were applied
to enhance the removal of air and water pollutants by photocatalytic degradation [3, 4]. Fe
2
O
3
-
clay nanocomposites were used to removal of dyes [5] and aromatic compounds [6].
In this work the TiO
2
- and Fe
2
O
3
- halloysite nanocomposites were prepared using halloysite
from “Dunino” mine (Legnica, Poland). These nanocomposites were synthesized using the sol-
gel method with titanium isopropoxide as a precursor of TiO
2
and gelatinous ferric hydroxide as
a ferric precursor under hydrothermal treatment at 65°C. Chemical and phase composition,
particle morphology, and physical properties of these nanocomposites were studied with the use
of wavelength dispersive X-ray fluorescence (WDXRF), X-ray diffraction (XRPD), X-ray
photoelectron spectroscopy (XPS), electron microscopy (TEM), FTIR technique, and UV-
VIS/DR spectra. TEM and XPS results confirmed good dispersion of TiO
2
and Fe
2
O
3
particles
on the halloysite surface, an increased content of titanium and iron in nanocomposite samples
was observed using WDXRF method. Determination of TiO
2
crystaline structure in the anatase
and rutile form, Fe
2
O
3
as hematite form was possible with XRPD method. The interactions of
oxides with surface of halloysite were proven based on FTIR spectra.
Keywords: halloysite; TiO
2
; Fe
2
O
3
; nanocomposite
References
[1] E. Joussein, S. Petit, G. J. Churchman, B. K. G. Theng, D. Righi, B. Delvaux, Clays Clay Miner. 40
(2005) 383.
[2] P. Yuan, D. Tan, F. Annabi-Bergaya, Appl. Clay Sci. 112–113 (2015) 75.
[3] D. Kibanova, M. Trejo, H. Destaillats, J. Cervini-Silva, Appl. Clay Sci. 42 (2009) 563.
[4] D. Papoulis, S. Komarneni, D. Panagiotaras, E. Stathatos, D. Toli, K.C. Christoforidis, M. Fernandez-
Garcia, H. Li, S. Yin, T. Sato, H. Katsuki, App. Catal. B: Environ. 132–133 (2013) 416.
[5] A.A. Tireli, I. do Rosário Guimarães, J.C. de Souza Terra, R.R. da Silva, M.C. Guerreiro, Environ.
Sci. Pollut. Res. 22 (2015) 870.
[6] M.M. Vianna, J. Dweck, F.H. Quina, F.M. Carvalho, C.A. Nascimento, J. Them. Anal. Calorim. 100
(2010) 889.
XIV
h
International Conference on Molecular Spectroscopy, Białka Tatrzańska 2017
169
T1: P–36
Hydroxyapatite molecules formation on titanium 99.2 substrates
after duplex/hybrid treatment
Jaroslaw Jan Jasinski
1
, Tadeusz Fraczek
2
, Małgorzata Lubas
2
,
Łukasz Kurpaska
3
, Jozef Jasinski
1
, and Maciej Sitarz
4
1
Czestochowa University of Technology, Institute of Logistics and International Management,
Av. Armii Krajowej 19, 42-200 Czestochowa, e-mail: jarjasinski@o2.pl
2
Czestochowa University of Technology, Institute for Materials Science, Av. Armii Krajowej 19,
42-200 Czestochowa,
3
Materials Research Laboratory, National Center for Nuclear Research, Swierk – Otwock 05-500,
Poland
4
AGH University of Science and Technology, Faculty of Materials Science and Ceramics,
Av. A.Mickiewicza 30, Krakow
The paper presents a structure of a layer nitride formed with active screen nitriding, which is
a modification of plasma nitriding. The model research material was Fe Armco. The nitriding
processes were carried out at 773K, 813K for different times and altering plasma parameters.
The results of the tests realized carried out were evaluated using scanning electron microscopy
(SEM, SEM/EBSD), transmission electron microscopy – electron energy loss spectroscopy
(TEM-EELS),
X-ray diffraction (GID – Grazing Incidence Diffraction), secondary ion mass spectroscopy
(SIMS) and X-ray photoelectron spectroscopy (XPS). The analysis of the results has confirmed
that the structures of the nitrided layers are different for various parameters and dependent on
the surface layer saturation mechanism in each of the temperatures and process parameters.
Effect of nitrogen transport in the layer was observed by several effects i.e. uphill diffusion
effect which confirms migration of atoms in diffusive layer towards top surface (ε-layer). The
knowledge on the structural components and nitrogen atoms migration and nitriding mechanism
made it possible to optimize nitriding parameters in order to reduce and even eliminate the
usually unfavourable, brittle nitrides and porous zones of the nitrided layer.
Keywords: Fe-armco; uphill diffusion; plasma nitriding; active screen technique
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