Kinetic Regularity of the Formation of Fe(II)–Fe(III) LDH Structures (Green Rust) on the Steel Surface in Presence of the FeSO4 and Fe2(SO4)3 Water Solutions
The kinetic regularity of origin and transformation of the Fe (II)–Fe (III) LDH structures on the steel electrodes surface contacting with FeSO4 and Fe2(SO4)3 dispersion medium at free access of the air oxygen into the system was studied. X-ray diffraction was chosen as the main method of investigat...
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Інститут хімії поверхні ім. О.О. Чуйка НАН України
2010
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| Zitieren: | Kinetic Regularity of the Formation of Fe(II)–Fe(III) LDH Structures (Green Rust) on the Steel Surface in Presence of the FeSO4 and Fe2(SO4)3 Water Solutions / O.M. Lavrynenko, Ya.D. Korol, S.V. Netreba, V.A. Prokopenko // Хімія, фізика та технологія поверхні. — 2010. — Т. 1, № 3. — С. 338-342. — Бібліогр.: 14 назв. — англ. |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1859687860210237440 |
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| author | Lavrynenko, O.M. Korol, Ya.D. Netreba, S.V. Prokopenko, V.A. |
| author_facet | Lavrynenko, O.M. Korol, Ya.D. Netreba, S.V. Prokopenko, V.A. |
| citation_txt | Kinetic Regularity of the Formation of Fe(II)–Fe(III) LDH Structures (Green Rust) on the Steel Surface in Presence of the FeSO4 and Fe2(SO4)3 Water Solutions / O.M. Lavrynenko, Ya.D. Korol, S.V. Netreba, V.A. Prokopenko // Хімія, фізика та технологія поверхні. — 2010. — Т. 1, № 3. — С. 338-342. — Бібліогр.: 14 назв. — англ. |
| collection | DSpace DC |
| container_title | Хімія, фізика та технологія поверхні |
| description | The kinetic regularity of origin and transformation of the Fe (II)–Fe (III) LDH structures on the steel electrodes surface contacting with FeSO4 and Fe2(SO4)3 dispersion medium at free access of the air oxygen into the system was studied. X-ray diffraction was chosen as the main method of investigation. It was shown that regardless of oxidation level of iron with its concentration 102–103 mg/dm3 on electrode surface the GR(SO4 2-) phase was formed staying single for almost 5 hours. The phase transformation of embryonic GR(SO4 2-) surface structures occur with formation of morphological composites of iron-oxygen g -row: lepidocrocite g -FeOOH and magnetite Fe3O4, and α-row structure representative, goethite α-FeOOH.
Досліджені кінетичні закономірності зародження та перетворення структур Fe (II)–Fe (III) шаруватих подвійних гідроксидів (ШПГ) на поверхні сталевого електрода, який контактує з дисперсійним середовищем, що містить FeSO4 та Fe2(SO4)3, за умови вільного надходження в систему кисню повітря. Головним методом дослідження був рентгенофазовий аналіз (РФА). Показано, що незалежно від ступеня окиснення заліза в дисперсійному середовищі при його концентрації 102–103 мг/дм3 на поверхні електроду утворюється фаза GR(SO4 2-), яка залишається єдиною протягом 5 годин. Фазові трансформації зародкових поверхневих структур GR(SO4 2-) проходять з утворенням залізокисневих структур g -ряду: лепідокрокіту g -FeOOH і магнетиту Fe3O4 та представника α-ряду, гетиту α-FeOOH.
Исследованы кинетические закономерности зарождения и трансформации структур Fe (II)-Fe (III) слоевых двойных гидроксидов (СДГ) на поверхности стального электрода, который контактирует с дисперсионной средой, содержащей FeSO4 и Fe2(SO4)3, при свободном доступе в систему кислорода воздуха. Основным методом исследования был рентгенофазовый анализ (РФА). Показано, что независимо от степени окисления железа в дисперсионной среде при его концентрации 102–103 мг/дм3 на поверхности электрода образуется фаза GR(SO4 2-), которая остается единственной в течение 5 часов. Фазовые трансформации зародышевых поверхностных структур GR(SO4 2-) проходят с образованием железо-кислородных структур γ-ряда: лепидокрокита γ-FeOOH и магнетита Fe3O4 и представителя α-ряда, гетита α-FeOOH.
|
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UDC 544.77+543.442.2
KINETIC REGULARITY OF THE FORMATION
OF Fe (II)–Fe (III) LDH STRUCTURES (GREEN RUST)
ON THE STEEL SURFACE IN PRESENCE OF THE FeSO4
AND Fe2(SO4)3 WATER SOLUTIONS
O.M. Lavrynenko1, Ya.D. Korol2, S.V. Netreba1, V.A. Prokopenko1
1Ovcharenko Institute of Bio-Colloid Chemistry of National Academy of Sciences of Ukraine
42 Vernadsky Ave., Kyiv 03142, Ukraine, ibcc@ukrpost.ua
2Khmelnitsky Cherkasy National University
81 Shevchenko Ave., Cherkasy18031, Ukraine, king@cdu.edu.ua
The kinetic regularity of origin and transformation of the Fe (II)–Fe (III) LDH structures on the
steel electrodes surface contacting with FeSO4 and Fe2(SO4)3 dispersion medium at free access of
the air oxygen into the system was studied. X-ray diffraction was chosen as the main method of investiga-
tion. It was shown that regardless of oxidation level of iron with its concentration 102–103 mg/dm3 on
electrode surface the GR(SO4
2-) phase was formed staying single for almost 5 hours. The phase
transformation of embryonic GR(SO4
2-) surface structures occur with formation of morphological
composites of iron-oxygen g-row: lepidocrocite g-FeOOH and magnetite Fe3O4, and � -row struc-
ture representative, goethite � -FeOOH.
INTRODUCTION
The present state of the chemistry science
has created conditions for close connection with
branches of knowledge which need the produc-
tion of new materials, for example, on the basis
of iron which can be used for the needs of biol-
ogy and medicine, particularly for creating mag-
netic carriers for controlled transport of a medi-
cal product in the magnetic field, the developing
new antioxidant protection of organism, creating
antitumoral preventive and therapeutic medicine,
etc. Fe (II)–Fe (III) LDH or Green Rust have got
magnetic [1] and reducing [2] properties and
they can transform to iron oxyhydroxides and
oxides of different crystallographic modifica-
tions [3] or ferrites by creating favorable condi-
tions of synthesis (oxidation conditions, chemi-
cal composition and pH meaning, addition of
stabilizing components and surface modifiers).
At the same time, reaction ability of such struc-
tures limits the time of their existence in stan-
dard conditions which might bring to difficulties
in LDH investigations and there is the necessity
of applying additional ways of their treatment
and stabilization [4]. Fe (II)–Fe (III) LDH struc-
tures are composed from hydroxides layers,
which are formed from octahedrons FeII-III (OH)6,
with interlayer water molecules and anions
which compensate the charge of Fe (III) hy-
droxides layers and supply electroneutrality of
the structure. In general, the structure of Green
Rust corresponds to the chemical composition
[FeII
(1-x)FeIII
x(OH)2]
x+ · [(x/nA·(m/n)H2O)]x- [5].
In laboratory, the Fe (II)–Fe (III) LDH structures
are obtained by chemical or electrochemical
techniques [6, 7].
Traditional investigation methods of Fe(II)–
Fe(III) LDH are M� ssbauer and Raman spec-
troscopy, X-ray diffraction, scanning electron
microscopy (SEM). The aim of our investigation
is studying the kinetic regularity of origin and
transformation of the Fe (II)–Fe (III) LDH struc-
tures on the steel electrodes surface contacting
with FeSO4 and Fe2(SO4)3 dispersion medium at
the condition of free access of the air oxygen
into the system.
MATERIALS AND METHODS
The studying of process Fe (II)–Fe (III)
LDH formation has been carried out on the sur-
face of the disk electrode from finished steel
(St3) with composition (%): � – 0.14–0.22;
Si – 0.05–0.15; Mn – 0.4–0.65; Cr – 0.3; Ni –
0.3; P – 0,04; S – 0,05; N – 0,01. The
Fe2(SO4)3·and FeSO4 solutions in pH range
Kinetic Regularity of the Formation of Fe(II)-Fe(III) LDH Structures (Green Rust)
_____________________________________________________________________________________________
���� 2010. � . 1. � 3 339
from 3.0 to 11.0 with Fe concentrations from
10 to 1·103 mg/dm3 have been chosen as disper-
sion medium. X-ray diffraction (XRD) was
chosen as the main method of investigation.
Measurement was taken on computer-aided
equipment (DRON 3) with filtered emission of
iron anode in discrete conditions of plotting
with pitch of 0.1 degree and time of piling in
every point 4 s. The addition module was used
for recording this process in situ. The rotation
of the steel disk supplied the variable contact of
their surface with air and dispersion medium.
The scanning electron microscopy (SEM) was
suggested as additional visualization technique
of the derived samples.
RESULTS AND DISCUSSION
The study of formation the embryonic struc-
tures of Fe (II)–Fe (III) LDH into Fe (II) and
Fe(III) sulfate solution shows the presence of
hydroxysulfate Green Rust II (GR(SO4
2-)) with
general composition FeII
4FeIII
2(OH)12SO4~8H2O
[8] after 10–20 min; spatial group of this struc-
ture is trigonal – 13mP ; parameters of elementary
lattice are a=0.55241 nm, c=1.10113 nm,
V=0.29097 nm3 and Z=1/2. Fig. 1 shows a
XRD-data of GR(SO4
2-) structure after 40 min
from the beginning of observation and additional
plot shows kinetic correspondence of intensity of
the most important characteristic picks 1.090 and
0.548 nm (planes (001) and (002), respectively).
10 30 50
200
400
600
2Q
1200
1000
800
600
400
0 2 4 6 8 10 12 14
200
Time, h
- 1 - 3
- 2 - 4
0
01
0
02
0
03
1
01
Fig. 1. XRD data of hydroxysulfate Green Rust
(GR(SO4
2-) sample: 1 – a-Fe0, 2 – GR(SO4
2-);
the kinetic of reflection intensity the planes of
GR(SO4
2-): 3 – (001), 4 – (002) on the addi-
tional graph
The formation of the GR(SO4
2-) structure
was ascertained in pH range from 3.0 to 11.0 by
the experimental investigation. Derived experi-
mental data show the growth of bulk of Green
Rust on the steel surface during 3–5 hours when
Fe (II) and Fe (III) salts with contents of cation
about 102–103 mg/dm3 were dissolved into dis-
tilled water. Than GR structures are transformed
into Fe (III) oxyhydroxides phases. The rate of
oxyhydroxides within of surface structures
grows and comes up to the maximum after
72 hours. At the extreme points of pH value the
formations of hydroxysulfate Green Rust II
(GR(SO4
2-) occurres in pittings. By lowering the
initial iron concentration to 10 mg/dm3 and
variating the pH value the formation of phase
GR(SO4
2-) is not always identified by XRD but
its presence was confirmed by SEM. In that
condition of carrying out the process the phase
consisting of surface structures is characterized
by the decreasing the relative quantity of phase
GR and increasing relative % mass the total
mass phase a- and g-iron oxyhydroxides and
magnetite. With it in Fe (II) system the inten-
siveness of growing GR phase and speed of that
process exceed twice that result as compared
with Fe (III) system.
Under the contact of the electrode surface
with dispersion medium the relative quantity of
magnetite Fe3O4 phase had come up to the
maximum in 24 hours and than decreased. The
total mass of iron oxyhydroxides, on the con-
trary, increases and after 72 hours of the ex-
periment makes up ~80% of the total mass of
surfaces of iron-oxygen structures. Fig. 2 shows
electronic microphotos of GR(SO4
2-) structures
which were obtained in neutral dispersion me-
dium on the surfaces of a steel electrode at con-
tacting with saturated air oxygen of dispersion
medium. The particles of Fe (II)–Fe (III) LDH
(size 0.5–1.0 � m) contact with one another and
participate in formation of solid layer on elec-
trode surfaces.
In accordance with the derived data an as-
sumption was made about the mechanism of the
processes of iron-oxygen structures formation on
the steel electrode surface which was contacting
with water dispersion medium and air oxygen.
During the first hours of the processing in the
thin films initial iron-oxygen structure is formed
on the surface containing the Fe (II) and Fe (III)
cations and according to the XRD-data corre-
sponding to hydroxysulfate Green Rust
(GR(SO4
2-). According to literature source [9],
the development of such a structure could occur
due to formation of goethite a-FeOOH phase by
oxidation Fe (II)–Fe (III) LDH with oxygen dis-
solved in dispersion medium. In our case this
process occurs as a result of the forced oxygen
O.M. Lavrynenko, Ya.D. Korol, S.V. Netreba, V.A. Prokopenko
_____________________________________________________________________________________________
340 ���� 2010. � . 1. � 3
delivering to electrode surface at the expense of
its rotating under changeable contact with air
and dispersion medium. Another typical process
was phase transformation of Green Rust into
lepidocrocite � -FeOOH [10]. As in [11], in both
cases the mechanism of phase transformation
could be divided into two stages – partial de-
struction of phase Green Rust and secondary
precipitated well ordered structures of iron (III)
oxyhydroxides.
a
b
Fig. 2. Structures of Fe (II)–Fe (III) layered double
hydroxide (GR(SO4
2-)) formed on the surface of
steel electrode by its contact with water disper-
sion medium at free access of air oxygen into
the system
The formation of magnetite phase at the be-
ginning of the process of structure formation,
according to [12], could occur by oxidation in
lattice of Fe (II)–Fe (III) LDH~33% Fe (II): in
that case phase of magnetite supplement or re-
place the structural elements of Green Rust. The
following oxidation of iron goes by destruction
of the phase magnetite Fe3O4 and Green Rust
and formation well-crystallizing needle-shaped
particles of lepidocrocite � -FeOOH [12]. In gen-
eral, the transformation of the structure
GR(SO4
2-) into the phases of iron (III) oxyhy-
droxides or magnetite could pass by the follow-
ing reactions
2FeII
4FeIII
2(OH)12SO4 + 1.5O2 �
� 10FeOOH +2FeSO4 + 7H2O
2FeOOH + Fe2+ + 2OH– � FeFe2O4 + 2H2O
(DG0
298 = -24.4 kcal/mol)
FeII
4FeIII
2(OH)12SO4 + 0.5O2 �
� 2Fe3O4 + H2SO4 + 5H2O
In its turn oxidation of the magnetite at the
expense of air oxygen facilitates the formation of
the iron oxyhydroxide
2FeFe2O4 + 0.5O2 + 3H2O �
� 6FeOOH (DG0
298= -49.7 kcal/mol).
Thus the replacement of oxidation condition
and entering the system by the hydroxyl ions and
Fe (II), for example by the passing electro-
chemical Red-Ox reaction on the steel surface,
gives an opportunity to control the process of
phase formation and to get separate phases
GR(SO4
2-), FeOOH or Fe3O4 on the steel sur-
face. In the same time, as a consequence of di-
rect interaction between the products of elec-
trode processes near-electrode space the forma-
tion of iron (II) hydroxide and its oxidation to
magnetite are possible [13]
6Fe(OH)2 + O2 �
� 2Fe3O4 + 6H2O (DG0
298= -123.0 kcal/mol)
or by oxidation Fe(OH)2 in presence of Fe (II)
and SO4
2- – to phase of GR(SO4
2-). As in [14],
such transformation has topotactical character,
i.e. the oxidation of Fe (II) occurs by partial re-
arrangement of Fe(OH)2 lattice without lattice
destruction
5Fe(OH)2+Fe2++SO4
2-+0.5O2+9H2O �
� FeII
4FeIII
2(OH)12SO4�8H2O
(DG0
298= -2522.1 kcal/mol).
However, in our case the formation of Fe(OH)2
was not seen.
Kinetic Regularity of the Formation of Fe(II)-Fe(III) LDH Structures (Green Rust)
_____________________________________________________________________________________________
���� 2010. � . 1. � 3 341
� ONCLUSIONS
The investigation of kinetic correspondence of
formation of the embryonic Fe (II)–Fe (III) LDH
structures (Green Rust) on the steel surface in
presence of the FeSO4 and Fe2(SO4)3 water solu-
tions was recorded in situ by X-ray diffraction. It
was shown that regardless of oxidation level of
iron with its concentration 102–103 mg/dm3 on
electrodes surface the phase GR(SO4
2-)was
formed and stayed single for almost 5 hours. A
change of the conditions of carrying out the proc-
ess resulted in considerable decrease of hydroxy-
sulfate Green Rust (GR(SO4
2-) emergence.
The phase transformation of embryonic sur-
faces structures GR(SO4
2-) occurs with formation
of morphological composites of iron-oxygen
g-row: lepidocrocite g-FeOOH and magnetite
Fe3O4 and � -row structure representative, goethite
� -FeOOH. Changing the physical-chemical con-
dition processing of phase formation, such as
quantity of oxidant which comes to electrode sur-
face, could change the way of the process going
to the side of formation of other iron-oxygen
structures.
ACKNOWLEDGEMENTS
The authors would like to express their grati-
tude to Dr. V. Nadutov, Dr. A Rud and PhD
O. Semyrga (Kurdumov Institute for Metal
Physics NAS of Ukraine) for informational and
technical help.
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Received 19.05.2010, accepted 17.08.2010
O.M. Lavrynenko, Ya.D. Korol, S.V. Netreba, V.A. Prokopenko
_____________________________________________________________________________________________
342 ���� 2010. � . 1. � 3
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| id | nasplib_isofts_kiev_ua-123456789-29004 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 2079-1704 |
| language | English |
| last_indexed | 2025-11-30T22:52:37Z |
| publishDate | 2010 |
| publisher | Інститут хімії поверхні ім. О.О. Чуйка НАН України |
| record_format | dspace |
| spelling | Lavrynenko, O.M. Korol, Ya.D. Netreba, S.V. Prokopenko, V.A. 2011-11-27T18:01:42Z 2011-11-27T18:01:42Z 2010 Kinetic Regularity of the Formation of Fe(II)–Fe(III) LDH Structures (Green Rust) on the Steel Surface in Presence of the FeSO4 and Fe2(SO4)3 Water Solutions / O.M. Lavrynenko, Ya.D. Korol, S.V. Netreba, V.A. Prokopenko // Хімія, фізика та технологія поверхні. — 2010. — Т. 1, № 3. — С. 338-342. — Бібліогр.: 14 назв. — англ. 2079-1704 https://nasplib.isofts.kiev.ua/handle/123456789/29004 544.77+543.442.2 The kinetic regularity of origin and transformation of the Fe (II)–Fe (III) LDH structures on the steel electrodes surface contacting with FeSO4 and Fe2(SO4)3 dispersion medium at free access of the air oxygen into the system was studied. X-ray diffraction was chosen as the main method of investigation. It was shown that regardless of oxidation level of iron with its concentration 102–103 mg/dm3 on electrode surface the GR(SO4 2-) phase was formed staying single for almost 5 hours. The phase transformation of embryonic GR(SO4 2-) surface structures occur with formation of morphological composites of iron-oxygen g -row: lepidocrocite g -FeOOH and magnetite Fe3O4, and α-row structure representative, goethite α-FeOOH. Досліджені кінетичні закономірності зародження та перетворення структур Fe (II)–Fe (III) шаруватих подвійних гідроксидів (ШПГ) на поверхні сталевого електрода, який контактує з дисперсійним середовищем, що містить FeSO4 та Fe2(SO4)3, за умови вільного надходження в систему кисню повітря. Головним методом дослідження був рентгенофазовий аналіз (РФА). Показано, що незалежно від ступеня окиснення заліза в дисперсійному середовищі при його концентрації 102–103 мг/дм3 на поверхні електроду утворюється фаза GR(SO4 2-), яка залишається єдиною протягом 5 годин. Фазові трансформації зародкових поверхневих структур GR(SO4 2-) проходять з утворенням залізокисневих структур g -ряду: лепідокрокіту g -FeOOH і магнетиту Fe3O4 та представника α-ряду, гетиту α-FeOOH. Исследованы кинетические закономерности зарождения и трансформации структур Fe (II)-Fe (III) слоевых двойных гидроксидов (СДГ) на поверхности стального электрода, который контактирует с дисперсионной средой, содержащей FeSO4 и Fe2(SO4)3, при свободном доступе в систему кислорода воздуха. Основным методом исследования был рентгенофазовый анализ (РФА). Показано, что независимо от степени окисления железа в дисперсионной среде при его концентрации 102–103 мг/дм3 на поверхности электрода образуется фаза GR(SO4 2-), которая остается единственной в течение 5 часов. Фазовые трансформации зародышевых поверхностных структур GR(SO4 2-) проходят с образованием железо-кислородных структур γ-ряда: лепидокрокита γ-FeOOH и магнетита Fe3O4 и представителя α-ряда, гетита α-FeOOH. The authors would like to express their gratitude to Dr. V. Nadutov, Dr. A Rud and PhD O. Semyrga (Kurdumov Institute for Metal Physics NAS of Ukraine) for informational and technical help. en Інститут хімії поверхні ім. О.О. Чуйка НАН України Хімія, фізика та технологія поверхні Неорганічні та вуглецеві наноматеріали і наносистеми Kinetic Regularity of the Formation of Fe(II)–Fe(III) LDH Structures (Green Rust) on the Steel Surface in Presence of the FeSO4 and Fe2(SO4)3 Water Solutions Кінетичні закономірності формування структур Fe (II)–Fe (III) ШПГ (Green Rust) на поверхні сталі в присутності водних розчинів FeSO4 та Fe2(SO4)3 Кинетические закономерности формирования структур Fe (II)-Fe (III) СДГ (Green Rust) на поверхности стали в присутствии водных растворов FeSO4 и Fe2(SO4)3 Article published earlier |
| spellingShingle | Kinetic Regularity of the Formation of Fe(II)–Fe(III) LDH Structures (Green Rust) on the Steel Surface in Presence of the FeSO4 and Fe2(SO4)3 Water Solutions Lavrynenko, O.M. Korol, Ya.D. Netreba, S.V. Prokopenko, V.A. Неорганічні та вуглецеві наноматеріали і наносистеми |
| title | Kinetic Regularity of the Formation of Fe(II)–Fe(III) LDH Structures (Green Rust) on the Steel Surface in Presence of the FeSO4 and Fe2(SO4)3 Water Solutions |
| title_alt | Кінетичні закономірності формування структур Fe (II)–Fe (III) ШПГ (Green Rust) на поверхні сталі в присутності водних розчинів FeSO4 та Fe2(SO4)3 Кинетические закономерности формирования структур Fe (II)-Fe (III) СДГ (Green Rust) на поверхности стали в присутствии водных растворов FeSO4 и Fe2(SO4)3 |
| title_full | Kinetic Regularity of the Formation of Fe(II)–Fe(III) LDH Structures (Green Rust) on the Steel Surface in Presence of the FeSO4 and Fe2(SO4)3 Water Solutions |
| title_fullStr | Kinetic Regularity of the Formation of Fe(II)–Fe(III) LDH Structures (Green Rust) on the Steel Surface in Presence of the FeSO4 and Fe2(SO4)3 Water Solutions |
| title_full_unstemmed | Kinetic Regularity of the Formation of Fe(II)–Fe(III) LDH Structures (Green Rust) on the Steel Surface in Presence of the FeSO4 and Fe2(SO4)3 Water Solutions |
| title_short | Kinetic Regularity of the Formation of Fe(II)–Fe(III) LDH Structures (Green Rust) on the Steel Surface in Presence of the FeSO4 and Fe2(SO4)3 Water Solutions |
| title_sort | kinetic regularity of the formation of fe(ii)–fe(iii) ldh structures (green rust) on the steel surface in presence of the feso4 and fe2(so4)3 water solutions |
| topic | Неорганічні та вуглецеві наноматеріали і наносистеми |
| topic_facet | Неорганічні та вуглецеві наноматеріали і наносистеми |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/29004 |
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