Золь-гель синтез,оптичні властивості, морфологія та фотокаталітична активність діоксид титанових плівок, модифікованих етаноламінами як джерело азоту
In this work the titania films modified with ethanolamines are synthesized by sol-gel method using two different routes. Introduction of template during sol ripening leading to the formation of porous structure and a single stage synthesis resulting in non-porous surface are proposed. The optical pr...
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Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine
2012
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Surface| _version_ | 1869291610533003264 |
|---|---|
| author | Linnik, O. P. Shestopal, N. O. Smirnova, N. P. Eremenko, A. M. Stanculescu, A. Socol, M. |
| author_facet | Linnik, O. P. Shestopal, N. O. Smirnova, N. P. Eremenko, A. M. Stanculescu, A. Socol, M. |
| author_institution_txt_mv | [
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},
{
"author": "N. O. Shestopal",
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},
{
"author": "N. P. Smirnova",
"institution": "Інститут хімії поверхні ім. О.О. Чуйка Національної академії наук України"
},
{
"author": "A. M. Eremenko",
"institution": "Інститут хімії поверхні ім. О.О. Чуйка Національної академії наук України"
},
{
"author": "A. Stanculescu",
"institution": "Національний інститут фізики матеріалів Румунської академії наук"
},
{
"author": "M. Socol",
"institution": "Національний інститут фізики матеріалів Румунської академії наук"
}
] |
| author_sort | Linnik, O. P. |
| baseUrl_str | |
| collection | OJS |
| datestamp_date | 2018-11-27T09:37:46Z |
| description | In this work the titania films modified with ethanolamines are synthesized by sol-gel method using two different routes. Introduction of template during sol ripening leading to the formation of porous structure and a single stage synthesis resulting in non-porous surface are proposed. The optical properties and calculated band-gap values of the films are presented. The titania particle size of the modified films is increased in comparison with the bare one as results of Root mean square (RMS) and Roughness average (Ra) values. The influence of the synthesis conditions and structure of ethanolamines on the photocatalytic activity under visible light are reported. |
| first_indexed | 2025-07-22T19:33:22Z |
| format | Article |
| fulltext |
Поверхность. 2012. Вып. 4(19). С. 91–98 91
ФИЗИКО‐ХИМИЯ ПОВЕРХНОСТНЫХ ЯВЛЕНИЙ
UDC 544.526+54.057
SOL-GEL SYNTHESIS, OPTICAL PROPERTIES,
MORPHOLOGY AND PHOTOCATALYTIC ACTIVITY OF
TITANIA FILMS MODIFIED WITH ETHANOLAMINES AS
NITROGEN SOURCE
O.P.Linnik1, N.O. Shestopal1, N.P. Smirnova1, A.М. Eremenko1,
A. Stanculescu2, M. Socol2
1Chuiko Institute of Surface Chemistry of National Academy of Sciences of Ukraine
17 General Naumov Str., Kyiv, 03164, Ukraine, okslinnik@yahoo.co.uk
2National Institute of Materials Physics
Atomistilor 105 bis Street, PO Box MG 07, Magurele, Romania
In this work the titania films modified with ethanolamines are synthesized by sol-gel method
using two different routes. Introduction of template during sol ripening leading to the formation of
porous structure and a single stage synthesis resulting in non-porous surface are proposed. The optical
properties and calculated band-gap values of the films are presented. The titania particle size of the
modified films is increased in comparison with the bare one as results of Root mean square (RMS) and
Roughness average (Ra) values. The influence of the synthesis conditions and structure of
ethanolamines on the photocatalytic activity under visible light are reported.
Introduction
Photocatalysts which are sensitive to visible light have been paid much attention for
their potential use of solar energy [1]. Nitrogen doped titania was first prepared by Sato [2]
calcinating titanium hydroxide with ammonium ions, after that the sensitization of TiO2
powders due to NOx impurities has been occurred. In particular, nitrogen-doped TiO2 is known
to be a promising photocatalyst sensitive to visible light [3]. Therefore, a number of studies on
the synthesis and characterization of various types of N-doped TiO2, including thin films [3-5],
single crystals [6] and powders [1, 7] has been reported. Based on theoretically calculation of
band energies, Asahi et al. [1] concluded that the substitution of nitrogen in the TiO2 lattice by
mixing the N 2p and O 2p state on the top of valence band could narrow the band gap energy.
The mechanism of band gap reduction is not clear due to the problem in locating the exact
position of N in the TiO2 lattice. However, XPS analysis claimed the state of doped nitrogen to
be N-anion [8], atomic β-nitrogen [9], and oxidation of TiN [10].
Mesoporous materials are getting considerable attention because of their potential
applications in the field of catalysis, bio-medical engineering, energy storage and conversion,
separation technology. Mesoporous titania is of particular interest due to photocatalytic and
photovoltaic applications [11, 12]. The preparation of mesoporous titania mainly relies on soft
template (supra molecular assemblies of surfactants or block copolymers) and hard template
(porous alumina, porous silica, porous carbon, polystyrene spheres) [13]. Template - free
approach based on different mechanisms was also developed to synthesize titania particles with
great activity [14].
We have attempted to prepare nitrogen doped titania from mono-, di-, and
triethanolamine by sol-gel method. The present paper deals with the synthesis of the nonporous
films by a soft chemical route that is template - free or a three-block copolymer of
polyethyleneoxide and polypropyleneoxide (PEO)20(PPO)70(PEO)20 (Pluronic P123) as a
92
template for the porous samples preparation. Since incorporated nitrogen release from titania
matrix as well as the acceleration of titania crystallization took place at above 500 °С [15], the
films were treated at 450 °C with heating rate 3 °C/min. The photocatalytic activity of the UV
and visible light active photocatalyst was evaluated towards the reduction of toxic Cr(VI) ions
as a model reaction.
Experimental
Titanium dioxide films were synthesized by sol-gel method and in detail described
herein [16]. The nitrogen containing films were synthesized by two procedures named as sol-
gel I and sol-gel II. All synthesis stages of sol-gel I were carried out analogous to bare titania
films with the final addition of doping agents (10 or 20 mol. %), namely, mono- (MEA), di-
(DEA) or triethanolamine (TEA). The entity of the sol-gel II was to add titanium isopropoxide (10
mol. %) to the previously heated (65 оС, water bath) doping agent with the following stirring of the
resulting mixture for 20 min. The one-layered films were deposited by dipping at the withdrawal rate of
1.5 mm/s onto previously cleaned glasses. Thermal treatment was carried at 450 оС with heating
rate of 3 оС/min.
Photocatalytic activity of the films was assessed via Cr(VI) ions reduction reaction. The
film was immersed in 40 ml of an aqueous solution of potassium bichromate (in all
experiments, the initial concentration of bichromate ions was 2*10-4 M) and the reducing agent
(disodium salt of ethylenediaminetetraacetic acid (Na2EDTA)) in the molar ratio 2:1 adjusted
to pH≥2 by perchloric acid. The reaction temperature was kept constant (20ºC) during the
experimental procedure. The change of Cr(VI) ions concentration was monitored with a
Lambda 35 UV-vis spectrophotometer (PerkinElmer) every 20 min at λ=350 nm. The distance
between the lamp and the reactor was set at 50 cm. For testing the visible light sensitivity, a
filter transmitting light with λ > 350 nm was introduced in the photocatalytic setup.
An irradiation source of UV light was 1000 W middle - pressure mercury lamp. The
absorption spectra of the films were recorded by a Lambda 35 UV-Vis spectrophotometer
(PerkinElmer) in the range of 200-1000 nm. AFM images were recorded using the microscope
is Nanonics Multiview 4000 with phase feedback, intermittent mode. Scanning area:
40mx40m; scan resolution: 256 lines; scanning speed: 6.12 lines/s; resonance frequency: 40
kHz; aperture diameter: 20 nm; active quality factor: 1600. The Nanonics Multiview 4000 is
working in tapped mode (intermittent contact) with a tuning fork probe with Cr/Au coating.
Results and discussion
To investigate the influence of nitrogen source and its amount on the optical properties
of the samples, the absorption spectra and band-gap values were obtained. The optical
absorbance of the films was determined by UV–vis spectroscopy and the band gap energies
(Eg) were calculated from the absorbance data.
As clearly seen the introduction of nitrogen containing compounds in concentration of
10 and 20 mol % to titania sol (sol-gel I) leads to the shift of absorption onset to the short
wavelengths (Fig. 1). It can be explained by the increase of band-gap (Eg) width due to anatase
particle size decrease [17] or the Burstein-Moss effect [18]. Such effect occurs in
semiconductors at the rising of dopant content and defines as the separation in energy between
the top of the valence band and the unoccupied energy states in the conduction band. The shift
arises because the Fermi energy (EF) lies in the conduction band for n-type doping (or in the
valence band for p-type doping). The filled states therefore block thermal or optical excitation.
Consequently the measured band gap determined from the onset of interband absorption moves
to higher energy.
93
300 350 400 450 500
0,00
0,25
0,50
0,75
1,00
Wavelength, nm
4
3
2
1
A
b
so
rb
a
n
ce
,
a
.u
.
350 400 450 500
0
1
4
3
2
1
A
bs
or
ba
nc
e
Wavelength, nm
Fig. 1. Absorption spectra of the films (sol-gel I) with 10% (a) and 20% (b) doping agent: 1
TiO2, 2-TiO2/DЕА, 3-TiO2/MЕА, 4-TiO2/ТЕА).
350 400 450 500 550 600
0,00
0,25
0,50
0,75
A
bs
or
ba
nc
e,
a
.u
wavelenght, nm
filter
1
2
3
Fig. 2. Absorption spectra of N/TiO2 films sol-gel ІІ: 1 - TiO2/MЕА, 2 - TiO2/TЕА and 3 -
TiO2/DЕА.
In opposite, the shift of absorption onset to the red region is observed for the films
synthesized by sol-gel II (Fig. 2). The narrowing of the band gap energy without any shift of
the conduction and valence bands position is considered an effect of N - generated mid-gap
level [19].
As follows, the optical absorption coefficient calculating from α = 4πk/λ can be used to estimate
the bad gap values of the samples. Indirect and direct transitions in a semiconductor can be
distinguished by the energy dependence of the optical absorption coefficient near the
absorption edge. The values of Eg for the samples with indirect and direct characteristics were
obtained by extrapolation of the plots of (αhv)1/2 and (αhv)2 versus hv, respectively. It has been
found from well distribution of experimental points that indirect electronic transition is
permitted for TiO2 as well as doped TiO2 films synthesized by us. The band gap values of indirect
electronic transition are in the range from 3.36 to 3.49 eV for doped samples and 3.42 eV for pure titania
film (Tab. 1).
94
Table 1. The band-gap values of the films for indirect electronic transitions
Eg, еV
sol-gel І
Sample
10% 20%
Eg, еV
sol-gel ІІ
ТіО2/МЕА 3.47 3.54 3.36
ТіО2/DЕА 3.44 3.36 3.49
ТіО2/ТЕА 3.45 3.42 3.36
ТіО2 3.42
The lowering in band-gap values is noted for the TiO2 films doped with 20 % BEA (sol-
gel I), MEA and TEA (sol-gel II). Such narrowing can be explained by the presence of
additional level above valence band as a result of nitrogen substitution for oxygen in the titania
structure.
a
Sol-gel I
b
Sol-gel II
c
d
e
Fig. 3. AFM images of the films synthesized by sol-gel I (left) and sol-gel II (right): TiO2 (a),
TiO2/DEA (b and c), TiO2/TEA (d and e).
For undoped TiO2 films we have evidenced a homogeneous, small-grain structure. By
the modification with ethanolamines the homogeneity of the film is affected. Well-pronounced
randomly distributed larger size crystallites developed on the film surface. The rough surface
texture is confirmed by the relatively higher values of the RMS. For the film containing DEA
the difference between the morphology of the films prepared by sol-gel I and sol-gel II is not
significant. For the films containing TEA the difference between the morphology of the films
prepared by sol-gel I and sol-gel II is important. For the modified titania, the biggest crystallite
size was obtained by the TEA modification using sol-gel II method.
The synthesized films were tested in photocatalytic reduction of bichromate ions in the
presence of sodium salt of EDTA at рН ≥ 2. Two blank experiments were carried out as the
catalytic reduction of dichromate ions (dark condition) and photoreduction reaction (a glass
substrate was used instead of a film). No significant changes in the absorption spectra of the
CrVI solution were observed for both blanks.
95
Table 3. RMS and Ra values of the films
Sample Root mean square (RMS) (nm) Roughness average (Ra)
(nm)
TiO2 5.28 3.99
TiO2/DEA (sol-gel II) 21.22 7.72
TiO2/TEA (sol-gel II) 13.44 9.76
TiO2/10%DEA (sol-gel I) 15.97 7.51
TiO2/10%TEA(sol-gel I) 19.22 9.83
The kinetics of the photocatalytic reduction under UV light showed that bare TiO2 film
exhibited higher activity in comparison with doped films where the first order reaction was
shown with reaction rate constant 11.9×10-5 s-1. In the case of doped samples, the zero order of
the reaction is observed and the calculated reaction rate constants are given in table 4. The
highest reaction rate under UV light is obtained for 10% МЕА/TiO2 film (sol-gel I) while other
tested films possessed the activity comparable to the blank. It can be explained by the
electronic structure modification due to the nitrogen incorporation. As follows, the
recombination of photogenerated electrons and holes are assisted by nitrogen doping leading to
the deceleration of bichromate ions reduction. A similar result is reported herein [20] where the
reaction rate of stearic acid photooxidation is lowered with the increasing of nitrogen content in
titania.
Table 4. The reaction rate constants of photocatalytic reduction of bichromate ions
Sample k×105
mol·L-1·s-1
k×106
mol·L-1·s-1
Exposed light UV Vis
Blank (glass) 2.4 4.0
TiO2 8.0
TiO2/10 % MEA
(sol-gel I)
5.1 4.2
TiO2/10 % DEA
(sol-gel I)
2.5 5.1
TiO2/10 % ТEA
(sol-gel I)
2.0 5.7
TiO2/20 % MEA
(sol-gel I)
1.6 6.3
TiO2/20 % DEA
(sol-gel I)
2.5 4.8
TiO2/20 % ТEA
(sol-gel I)
1.6 7.1
TiO2/MEA
(sol-gel II)
2.5 8.0
TiO2/DEA
(sol-gel II)
3.6 10.0
TiO2/ТEA
(sol-gel II)
2.7 8.8
When comparing the reaction rate constants under visible light, the films synthesized by sol-gel
I are found to be less active than TiO2. In opposite, the insignificant increase of reaction rates is
96
observed for doped TiO2 films synthesized by sol-gel II. Among them, the film with DEA
possessed the highest activity. It must be noted that the concurrent intensity decrease at 350 nm
and increase at 550 nm characterizing the formation as a product of non-toxic Cr(III) ions are
observed in the presence of such doped titania films. The significant absorption in visible
region is demonstrated by the TiO2/DEA and TiO2/ТEA films (Fig. 2) although the band gap
value of TiO2/DEA is too high to absorb the light with energy less than 3.5 eV. We expect that
exactly this evidence is responsible for improved photocatalytic activity of TiO2/DEA film.
Conclusions
The optically transparent nitrogen doped titania thin films have been synthesized by sol-
gel approach using various amount of MEA, DEA and TEA as doping agent. It was also
applied the technologically more simple route (sol-gel II) of film synthesis. Titania and doped
titania films showed the indirect electronic transition found from optical dependencies. The
surface morphology of doped films is differed from bare titania. The growth of anatase
crystallite sizes in the presence of ethanolamines has been observed. As shown TiO2/DEA (sol-
gel II) films are perspective in photocatalytic reduction of bichromate ions under visible light.
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98
ЗОЛЬ-ГЕЛЬ СИНТЕЗ,ОПТИЧНІ ВЛАСТИВОСТІ, МОРФОЛОГІЯ ТА
ФОТОКАТАЛІТИЧНА АКТИВНІСТЬ ДІОКСИД ТИТАНОВИХ ПЛІВОК,
МОДИФІКОВАНИХ ЕТАНОЛАМІНАМИ ЯК ДЖЕРЕЛО АЗОТУ
О.П. Ліннік1, Н.О. Шестопаль1, Н.П. Смірнова1, А.М. Еременко1,
A. Станкулеску2, M. Сокол2
1Інститут хімії поверхні ім.. O.O. Чуйка Національної академії наук України
вул. Генерала Наумова 17, Київ, 03164, Україна
2Національний інститут фізики матеріалів Румунської академії наук
вул. Атомістіор 105t, PO Box MG 07, Магуреле, Румунія
Синтезовано плівки діоксиду титану, модифіковані етаноламінами. Описано золь-гель
метод з використанням різних підходів. Введення темплату під час дозрівання золю призводить
до утворення пористої структури, а запропонований одностадійний синтез формує непористу
поверхню. Досліджено оптичні властивості плівок та розраховано їхні величини ширини
забороненої зони. Розмір частинок модифікованих плівок діоксиду титану зростає в порівнянні
з немодифікованим, як показано представленими значеннями RMS і Ra. Вивчено вплив умов
синтезу і структури етаноламінів на фотокаталітичну активність під видимим світлом.
ЗОЛЬ-ГЕЛЬ СИНТЕЗ,ОПТИЧЕСКИЕ СВОЙСТВА, МОРФОЛОГИЯ И
ФОТОКАТАЛИТИЧЕСКАЯ АКТИВНОСТЬ ДИОКСИД ТИТАНОВЫХ ПЛЕНОК,
МОДИФИЦИРОВАННЫХ ЭТАНОЛАМИНАМИ КАК ИСТОЧНИК АЗОТА
О.П. Линник1*, Н.А. Шестопаль1, Н.П. Смирнова1, А.М. Еременко1,
A. Станкулеску2, M. Сокол2
1Институт химии поверхности им. O.O. Чуйко Национальной академии наук Украины
ул. Генерала Наумова 17, Киев, 03164, Украина
2Национальний институт физики материалов Румынской академии наук
ул. Атомистиор 105t, PO Box MG 07, Магуреле, Румыния
.
В данной работе синтезированы пленки диоксида титана, модифицированные
этаноламинами. Описан золь-гель метод с использованием различных. Введение темплата во
время созревания золя приводит к образованию пористой структуры, а предложенный
одностадийный синтез формирует непористую поверхность. Исследованы оптические
свойства пленок и рассчитаны их величины ширины запрещенной зоны. Размер частиц
модифицированных пленок диоксида титана возрастает по сравнению с немодифицированным,
как показано представленными значениями RMS и Ra. Изучено влияние условий синтеза и
структуры этаноламинов на фотокаталитическую активность под видимым светом.
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| id | oai:ojs.pkp.sfu.ca:article-474 |
| institution | Surface |
| keywords_txt_mv | keywords |
| language | English |
| last_indexed | 2026-03-12T17:13:00Z |
| publishDate | 2012 |
| publisher | Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine |
| record_format | ojs |
| resource_txt_mv | surfacezbircomua/d0/7046b61fa75abb6c55029a459ac653d0.pdf |
| spelling | oai:ojs.pkp.sfu.ca:article-4742018-11-27T09:37:46Z Sol-gel synthesis, optical properties, morphology and photocatalytic activity of titania films modified with ethanolamines as nitrogen source Золь-гель синтез,оптические свойства, морфология и фотокаталитическая активность диоксид титановых пленок, модифицированных этаноламинами как источник азота Золь-гель синтез,оптичні властивості, морфологія та фотокаталітична активність діоксид титанових плівок, модифікованих етаноламінами як джерело азоту Linnik, O. P. Shestopal, N. O. Smirnova, N. P. Eremenko, A. M. Stanculescu, A. Socol, M. In this work the titania films modified with ethanolamines are synthesized by sol-gel method using two different routes. Introduction of template during sol ripening leading to the formation of porous structure and a single stage synthesis resulting in non-porous surface are proposed. The optical properties and calculated band-gap values of the films are presented. The titania particle size of the modified films is increased in comparison with the bare one as results of Root mean square (RMS) and Roughness average (Ra) values. The influence of the synthesis conditions and structure of ethanolamines on the photocatalytic activity under visible light are reported. В данной работе синтезированы пленки диоксида титана, модифицированные этаноламинами. Описан золь-гель метод с использованием различных. Введение темплата во время созревания золя приводит к образованию пористой структуры, а предложенный одностадийный синтез формирует непористую поверхность. Исследованы оптические свойства пленок и рассчитаны их величины ширины запрещенной зоны. Размер частиц модифицированных пленок диоксида титана возрастает по сравнению с немодифицированным, как показано представленными значениями RMS и Ra. Изучено влияние условий синтеза и структуры этаноламинов на фотокаталитическую активность под видимым светом. Синтезовано плівки діоксиду титану, модифіковані етаноламінами. Описано золь-гель метод з використанням різних підходів. Введення темплату під час дозрівання золю призводить до утворення пористої структури, а запропонований одностадійний синтез формує непористу поверхню. Досліджено оптичні властивості плівок та розраховано їхні величини ширини забороненої зони. Розмір частинок модифікованих плівок діоксиду титану зростає в порівнянні з немодифікованим, як показано представленими значеннями RMS і Ra. Вивчено вплив умов синтезу і структури етаноламінів на фотокаталітичну активність під видимим світлом. Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine 2012-09-04 Article Article application/pdf https://surfacezbir.com.ua/index.php/surface/article/view/474 Surface; No. 4(19) (2012): Surface; 91-98 Поверхность; № 4(19) (2012): Поверхность; 91-98 Поверхня; № 4(19) (2012): Поверхня; 91-98 3154-8091 3154-8083 en https://surfacezbir.com.ua/index.php/surface/article/view/474/473 Авторське право (c) 2012 O.P.Linnik, N.O. Shestopal, N.P. Smirnova, A.М. Eremenko, A. Stanculescu, M. Socol |
| spellingShingle | Linnik, O. P. Shestopal, N. O. Smirnova, N. P. Eremenko, A. M. Stanculescu, A. Socol, M. Золь-гель синтез,оптичні властивості, морфологія та фотокаталітична активність діоксид титанових плівок, модифікованих етаноламінами як джерело азоту |
| title | Золь-гель синтез,оптичні властивості, морфологія та фотокаталітична активність діоксид титанових плівок, модифікованих етаноламінами як джерело азоту |
| title_alt | Sol-gel synthesis, optical properties, morphology and photocatalytic activity of titania films modified with ethanolamines as nitrogen source Золь-гель синтез,оптические свойства, морфология и фотокаталитическая активность диоксид титановых пленок, модифицированных этаноламинами как источник азота |
| title_full | Золь-гель синтез,оптичні властивості, морфологія та фотокаталітична активність діоксид титанових плівок, модифікованих етаноламінами як джерело азоту |
| title_fullStr | Золь-гель синтез,оптичні властивості, морфологія та фотокаталітична активність діоксид титанових плівок, модифікованих етаноламінами як джерело азоту |
| title_full_unstemmed | Золь-гель синтез,оптичні властивості, морфологія та фотокаталітична активність діоксид титанових плівок, модифікованих етаноламінами як джерело азоту |
| title_short | Золь-гель синтез,оптичні властивості, морфологія та фотокаталітична активність діоксид титанових плівок, модифікованих етаноламінами як джерело азоту |
| title_sort | золь-гель синтез,оптичні властивості, морфологія та фотокаталітична активність діоксид титанових плівок, модифікованих етаноламінами як джерело азоту |
| url | https://surfacezbir.com.ua/index.php/surface/article/view/474 |
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