Obtaining and Spectrophotometric Study of Organic Solutions of C₆₀ Endo- and Exometallofullerenes
The method of ion-implantation synthesis of endo- and exofullerenes is developed. The samples of fullerenes containing iron, platinum or their mixture are prepared. Spectrophotometric investigations of low-concentration solutions of metallofullerenes dissolved in organic solvents (toluene) are carri...
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Інститут металофізики ім. Г.В. Курдюмова НАН України
2010
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| Cite this: | Obtaining and Spectrophotometric Study of Organic Solutions of C₆₀ Endo- and Exometallofullerenes / B.V. Borts, V.I. Tkachenko, A.V. Moskvitin, Yu.G. Kazarinov // Наносистеми, наноматеріали, нанотехнології: Зб. наук. пр. — К.: РВВ ІМФ, 2010. — Т. 8, № 1. — С. 185-192. — Бібліогр.: 13 назв. — англ. |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1859896911338668032 |
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| author | Borts, B.V. Tkachenko, V.I. Moskvitin, A.V. Kazarinov, Yu.G. |
| author_facet | Borts, B.V. Tkachenko, V.I. Moskvitin, A.V. Kazarinov, Yu.G. |
| citation_txt | Obtaining and Spectrophotometric Study of Organic Solutions of C₆₀ Endo- and Exometallofullerenes / B.V. Borts, V.I. Tkachenko, A.V. Moskvitin, Yu.G. Kazarinov // Наносистеми, наноматеріали, нанотехнології: Зб. наук. пр. — К.: РВВ ІМФ, 2010. — Т. 8, № 1. — С. 185-192. — Бібліогр.: 13 назв. — англ. |
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| description | The method of ion-implantation synthesis of endo- and exofullerenes is developed. The samples of fullerenes containing iron, platinum or their mixture are prepared. Spectrophotometric investigations of low-concentration solutions of metallofullerenes dissolved in organic solvents (toluene) are carried out. As shown, the bonding of metal atoms to the fullerene leads to the broadening of the absorption-spectrum line width and to the absorption-maximum shift to the long-wave part of the spectrum. The half-width and the shift are increasing in the series of С₆₀—С₆₀ + Pt—С₆₀ + Fe—С₆₀ + Fe + Pt.
Розроблено методику синтези ендо- та екзофуллеренів методою йонної імплантації. У цей спосіб було створено зразки фуллеренів, що містять залізо, плятину або їхню суміш. Виконані спектрофотометричні дослідження розчинів металофуллеренів малої концентрації в органічних розчинниках (толуолі) показали, що зв’язок атомів металу із фуллереном спричиняє розширення смуг у спектрах оптичного вбирання та зсув максимумів цих смуг у бік довгих хвиль. Півширина смуги та величина зсуву збільшується у ряду С₆₀—С₆₀ + Pt—С₆₀ + Fe—С₆₀ + Fe + Pt.
Разработана методика получения эндо- и экзофуллеренов методом ионной имплантации. Проведены спектрофотометрические исследования растворов малых концентраций полученных металлофуллеренов в органических растворителях. Показано, что присоединение к фуллерену атома металла приводит к увеличению ширины линий в спектре поглощения и смещению максимума поглощения в длинноволновую часть спектра. При этом полуширина и смещение увеличиваются в ряду С₆₀—С₆₀ + Pt—С₆₀ + Fe—С₆₀ + Fe + Pt.
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185
PACS numbers: 07.60.Dq, 61.72.up, 68.49.Sf, 78.40.Ri, 81.05.ub, 81.07.Nb, 81.15.Cd
Obtaining and Spectrophotometric Study of Organic Solutions
of C60 Endo- and Exometallofullerenes
B. V. Borts, V. I. Tkachenko, A. V. Moskvitin, and Yu. G. Kazarinov
National Scientific Centre ‘Kharkiv Institute of Physics and Technology’,
1, Academichna Str.,
61108 Kharkiv, Ukraine
The method of ion-implantation synthesis of endo- and exofullerenes is devel-
oped. The samples of fullerenes containing iron, platinum or their mixture are
prepared. Spectrophotometric investigations of low-concentration solutions of
metallofullerenes dissolved in organic solvents (toluene) are carried out. As
shown, the bonding of metal atoms to the fullerene leads to the broadening of
the absorption-spectrum line width and to the absorption-maximum shift to
the long-wave part of the spectrum. The half-width and the shift are increasing
in the series of С60—С60 + Pt—С60 + Fe—С60 + Fe + Pt.
Розроблено методику синтези ендо- та екзофуллеренів методою йонної
імплантації. У цей спосіб було створено зразки фуллеренів, що містять
залізо, плятину або їхню суміш. Виконані спектрофотометричні дослі-
дження розчинів металофуллеренів малої концентрації в органічних роз-
чинниках (толуолі) показали, що зв’язок атомів металу із фуллереном
спричиняє розширення смуг у спектрах оптичного вбирання та зсув мак-
симумів цих смуг у бік довгих хвиль. Півширина смуги та величина зсуву
збільшується у ряду С60—С60 + Pt—С60 + Fe—С60 + Fe + Pt.
Разработана методика получения эндо- и экзофуллеренов методом ионной
имплантации. Проведены спектрофотометрические исследования раство-
ров малых концентраций полученных металлофуллеренов в органиче-
ских растворителях. Показано, что присоединение к фуллерену атома ме-
талла приводит к увеличению ширины линий в спектре поглощения и
смещению максимума поглощения в длинноволновую часть спектра. При
этом полуширина и смещение увеличиваются в ряду С60—С60 + Pt—С60 + Fe—
С60 + Fe + Pt.
Key words: fullerenes, С60—С60 + Pt—С60 + Fe—С60 + Fe + Pt, implantation syn-
thesis, absorption spectrum.
(Received November 25, 2009)
Наносистеми, наноматеріали, нанотехнології
Nanosystems, Nanomaterials, Nanotechnologies
2010, т. 8, № 1, сс. 185—192
© 2010 ІМФ (Інститут металофізики
ім. Г. В. Курдюмова НАН України)
Надруковано в Україні.
Фотокопіювання дозволено
тільки відповідно до ліцензії
186 B. V. BORTS, V. I. TKACHENKO, A. V. MOSKVITIN, and Yu. G. KAZARINOV
1. INTRODUCTION
One of unique properties of fullerene molecules is an ability to contain
trapped atoms and molecules of other elements within their carbon cage.
The state of atomic particles, entrapped within the fullerene shell, is pe-
culiar and cannot be reproduced in a different way. Our interest con-
cerns endohedral and exohedral fullerenes containing, inside or outside,
atoms of other metals. Compounds of fullerenes with atoms of inert gas-
es and nitrogen attract lesser attention than metallofullerenes, as the
interaction between the endohedral atoms and the carbon cage is weak
and compounds obtained do not possess new specific properties.
Interest in fabrication of a wide range of endo- and exohedral metal-
lofullerenes [1—5] is aroused by particular properties of such-type ele-
ments, namely:
– feature of the electronic structure of endometallofullerenes related
with the transfer of metal valence electrons to the fullerene shell;
– endofullerenes containing atoms of the second-group metals possess
diamagnetic properties, since the entrapped two-charge metal ion con-
tains only fully occupied electron shells, and the spin moments of va-
lence electrons being on the external orbitals of the fullerene shell are
completely compensated;
– endofullerenes containing atoms of the third-group metals possess
paramagnetic properties since the entrapped three-charged metal ion
transfers three electrons onto the fullerene shell;
– displacement of a metal atom relatively to the geometric centre of
the molecule is related with transfer of valence electrons from the en-
trapped atom onto the outer surface of the fullerene shell;
– displacement of the equilibrium position of the entrapped atom
causes the presence of a rather significant constant dipole moment in
such molecule and the constant polarizability occurrence;
– presence of electrons on the external surface of the fullerene shell
determines the character of intermolecular interactions in the crystal,
which receives contributions from the Van der Waals mechanism and
from the covalent one;
– endofullerenes show ability to the orientation arrangement that
gives anisotropic properties to the fullerene-based crystals, making
them a promising material in for various applications.
At present, the opportunity to apply endohedral structures directly
in the technology and technique of physical experiment is rather lim-
ited, first, because of extremely high cost of their production [6].
The method of ion implantation synthesis of endohedral fullerenes is
based on the bombardment of empty fullerenes with ions of the element
that should be implanted into the carbon cage of a fullerene molecule or
are bonding with the outside of the cage by the electron couplings. How-
ever, to obtain accelerated metal ions, it is necessary to create an ion
source capable to produce ions, desirably all ions from the Periodic Ta-
ORGANIC SOLUTIONS OF C60 ENDO- AND EXOMETALLOFULLERENES 187
ble, which is a very difficult problem. The second problem is that for all
ion sources, as a rule, a beam mass separator is required, and the energy
obtained at the ion injector output is in the range of 20—30 keV. With
such energy, the incoming metal ion will break down electron couplings,
knockout carbon atoms from the lattice and will not establish necessary
fullerene couplings. The energy necessary for production of endo- and
exofullerenes is in the range of 10—100 eV. For intercalation of metal
atom, the energy should be selected so that the metal atom can approach
to the fullerene molecule. Then, this atom will bond with the carbon
atom outside the cage and establish the electron couplings with it, or
will open one of the electron couplings and penetrate into the carbon
cage, and the disturbed coupling will be re-established after that.
2. FABRICATION OF METALLOFULLERENES
On the assumption of the above-mentioned conditions, we have devel-
oped an installation (Fig. 1) capable to perform the fullerene intercala-
tion using any metal atoms. To obtain a flux of metal atoms, we use an
ion source producing an ion beam from the inert gases (argon or xenon)
with energies from 10 to 30 keV and a current to 100 μA. The beam is
directed at an angle from 0° to 85° onto the metal support and, as a re-
sult of its sputtering, the flux of metal atoms with energies from 10 to
100 eV is formed there.
Under the action of inert gases with energies from 10 to 30 keV, the
diffused atoms have a wide energy distribution on the metal target sur-
face with a maximum near the low values of kinetic energy (Fig. 2) [7].
Irradiating the metals under different angles, it is possible to sepa-
rate the maxima of angle distribution of high-energy reflected particles
of inert gas and the diffused particles of the target with energies suffi-
cient for metal ion implantation into the fullerene molecule (Fig. 3) [8].
In connection with a low probability for the output of sputtered parti-
Fig. 1. Installation for metal-ion sputtering onto the fullerite.
188 B. V. BORTS, V. I. TKACHENKO, A. V. MOSKVITIN, and Yu. G. KAZARINOV
cles with energies sufficient to break up fullerenes, the given method can
be used for effective production of endo- and exofullerene compounds.
The machine was used for intercalation fullerenes with iron (99.99%
purity) or platinum atoms as well as with iron and platinum together.
Fullerenes were extracted from the soot synthesized in the helium me-
dium by the vacuum arc method. The values of pressure (100—200 Torr)
and arc current (60—70 А) were determined by the optimum yield of
10−1 100 101 102 103
10−7
10−6
10−5
10−4
10−3
10−2
1
2
3
4
5
6
E−2
1 Xe+ 20 keV
2 Kr+ 20 keV
3 Kr+ 10 keV
4 Ar+ 20 keV
5 He+ 20 keV
6 D+ 20 keV
Energy, eV
d
2
S
/d
E
d
Ω
,
àò
îì
/(
io
n
⋅e
V
⋅s
ra
d
)
Fig. 2. Energy distribution of sputtered atoms from the crystalline gold target
by different ions.
5
0.1
5 5 5
1.0 10
Energy, keV
2
5
2
5
2
5
2
5
2
10−2
10−1
100
10
Y
Ar+
He+
Fig. 3. Experimental values of Pt sputtering yield.
ORGANIC SOLUTIONS OF C60 ENDO- AND EXOMETALLOFULLERENES 189
fullerenes. Extraction of fullerenes from the soot was performed with
the use of a laboratory facility comprising a standard Soxhlet’s appara-
tus and rotary evaporator modified by the vacuum pumping. The latter
decreases significantly the temperature of boiling solvent.
The fullerene compound was separated by the method of liquid-solid
adsorption chromatography in the chromatographic column filled with
graphite or Al2O3. The column has a valve controlling the eluent inflow
rate. Toluene or toluene mixed with hexane was used as an eluent. The
synthesized fullerene crystals were put on the watch crystal for treat-
ment with metal atoms or were dissolved in the little amount of toluene
and then were dried on the watch crystal in the drying chamber.
3. SPECTROPHOTOMETRIC STUDY OF ORGANIC SOLUTIONS
OF C60 ENDO- AND EXOMETALFULLERENES
The spectrophotometric method [9] can be applied for identification of
metallofullerenes prepared. This method provides much information
about the interaction between modified fullerenes and solvent molecules
[10, 11]. A metal atom implanted inside or bonded outside of the fullerene
molecule forms couplings with carbon atoms and substantially changes
the electronic and other properties of the molecule that influences on the
position and width of bands in the molecule absorption spectrum. Purifi-
cation (separation) of metallofullerenes was not specially carried out,
therefore С60 endo- and exometallofullerenes, slightly changing the ab-
sorption spectra, made an insignificant part in the total number of ful-
lerenes. However, these changes can be observed by the method of optical
spectrometry of diluted organic solutions of metallofullerenes.
Earlier, we have studied the optical spectra of organic solutions of
pure fullerenes synthesized in laboratory using the vacuum-arc instal-
lation [2]. Similar samples of pure fullerenes С60 were used as a target
for irradiation with atoms and ions of sputtered metals. The absorp-
tion spectra of pure fullerenes were standards in the spectrophotomet-
ric investigations of organic solutions of С60 endo- and exometallo-
fullerenes, prepared in the present work.
The spectrophotometric methods are the most advanced in techno-
logical studies for which the rapidity, low cost of measurements, and
little amounts of the material investigated are important factors.
Comparison between the absorption spectra of thin (10—100 μm) ful-
lerene films formed in vacuum [13] and the absorption spectra of high-
ly diluted (10—100 μg/ml) fullerene solutions demonstrates a similar
behaviour of absorption spectra in the range of 180—600 nm. Such thin
fullerene films should be investigated in the inert medium, as in the
oxygen-containing atmosphere fullerenes are oxidized to exohedral
forms. Highly-diluted fullerene solutions (of 10—100 μg/ml) allow sta-
ble working in the oxygen-containing atmosphere as the solvent pro-
190 B. V. BORTS, V. I. TKACHENKO, A. V. MOSKVITIN, and Yu. G. KAZARINOV
tects fullerenes from the interaction with oxygen and other gases. The
fact that the absorption spectra of fullerenes and diluted fullerene so-
lutions are identical can give nontrivial theoretical interpretations and
should be considered separately.
In a given work, we have carried out measurements of the absorption
spectra of solutions of fullerenes C60, C60 + Fe, C60 + Pt, and C60 + Fe + Pt
by means of a SF-2000 spectrometer in toluene at room temperature.
The initial solutions (of concentrations presented in Table 1) were di-
luted with toluene to obtain the optical solution density of an order of
unit.
Figure 4 presents the absorption spectra of metallofullerenes and pure
fullerenes С60. Comparison of the absorption spectra obtained for differ-
ent metals proves, despite the difference between the atomic mass and
the charge of trapped atoms, the validity of an empiric rule that absorp-
tion spectra of toluene solutions of different C60 + Me are identical [13].
Figure 5 shows an enlarged image of the spectral region near the
peak of 335 nm (3.7 eV) after normalization and smoothing. As seen,
because of fullerene treatment with metal ions, the peak position of the
optical density and the width of maximum are varying.
�
�
� �
Fig. 4. Absorption spectra of metallofullerenes and С60.
TABLE 1. Initial concentrations of the fullerene solutions investigated.
Sample Concentration
of an undiluted sample, mg/ml
Accuracy, %
С60 0.44 4.7
С60 + Pt 0.16 4.6
С60 + Fe 1.15 1.9
С60 + Pt + Fe 0.71 2.9
ORGANIC SOLUTIONS OF C60 ENDO- AND EXOMETALLOFULLERENES 191
The metal influence on the optical spectra of fullerenes was studied
by decomposition of normalized spectra into the components in the
form of Gaussian profiles.
Detailed analysis has shown that the peak form is insignificantly
changing under iron ion action (Fig. 6, a), while heavier platinum ions
�
�
� �
Fig. 5. Region near the peak of absorption spectra of metallofullerenes and
С60 after normalization and smoothing.
�
�
� �
a b
Fig. 6. Absorption spectra of fullerenes (thick lines) and C60 decomposed
into components (thin lines).
TABLE 2. Peak energy and width of fullerene solutions under consideration.
Sample Energy, eV FWHM, eV
С60 3.712 0.213
С60 + Pt 3.710 0.223
С60 + Fe 3.696 0.231
С60 + Pt + Fe 3.702 0.246
192 B. V. BORTS, V. I. TKACHENKO, A. V. MOSKVITIN, and Yu. G. KAZARINOV
lead to the peak deformation (Fig. 6, b). Parameters of the main peak
are given in Table 2 in the order of full width broadening at half-
maximum (FWHM) of peak.
The influence of platinum on the optical properties of fullerenes is
less as compared to iron and has an effect, for the most part, on the main
peak width, while the peak of iron-containing fullerenes is more shifted.
4. CONCLUSIONS
The method of ion implantation synthesis of endo- and exofullerenes
was developed. The samples of fullerenes containing iron, platinum, or
their mixture were prepared. Spectrophotometric investigations of
low-concentration solutions of fullerenes dissolved in organic solvents
(toluene) were carried out. As demonstrated, the bonding of a metal
atom to the fullerene leads to the broadening of the absorption-
spectrum line-width and to the absorption-maximum shift to the long-
wave part of the spectrum. The half-width and the shift are increasing
in the series of С60—С60 + Pt—С60 + Fe—С60 + Fe + Pt.
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|
| id | nasplib_isofts_kiev_ua-123456789-72477 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1816-5230 |
| language | English |
| last_indexed | 2025-12-07T15:54:45Z |
| publishDate | 2010 |
| publisher | Інститут металофізики ім. Г.В. Курдюмова НАН України |
| record_format | dspace |
| spelling | Borts, B.V. Tkachenko, V.I. Moskvitin, A.V. Kazarinov, Yu.G. 2014-12-23T21:59:17Z 2014-12-23T21:59:17Z 2010 Obtaining and Spectrophotometric Study of Organic Solutions of C₆₀ Endo- and Exometallofullerenes / B.V. Borts, V.I. Tkachenko, A.V. Moskvitin, Yu.G. Kazarinov // Наносистеми, наноматеріали, нанотехнології: Зб. наук. пр. — К.: РВВ ІМФ, 2010. — Т. 8, № 1. — С. 185-192. — Бібліогр.: 13 назв. — англ. 1816-5230 PACS numbers: 07.60.Dq, 61.72.up, 68.49.Sf, 78.40.Ri, 81.05.ub, 81.07.Nb, 81.15.Cd https://nasplib.isofts.kiev.ua/handle/123456789/72477 The method of ion-implantation synthesis of endo- and exofullerenes is developed. The samples of fullerenes containing iron, platinum or their mixture are prepared. Spectrophotometric investigations of low-concentration solutions of metallofullerenes dissolved in organic solvents (toluene) are carried out. As shown, the bonding of metal atoms to the fullerene leads to the broadening of the absorption-spectrum line width and to the absorption-maximum shift to the long-wave part of the spectrum. The half-width and the shift are increasing in the series of С₆₀—С₆₀ + Pt—С₆₀ + Fe—С₆₀ + Fe + Pt. Розроблено методику синтези ендо- та екзофуллеренів методою йонної імплантації. У цей спосіб було створено зразки фуллеренів, що містять залізо, плятину або їхню суміш. Виконані спектрофотометричні дослідження розчинів металофуллеренів малої концентрації в органічних розчинниках (толуолі) показали, що зв’язок атомів металу із фуллереном спричиняє розширення смуг у спектрах оптичного вбирання та зсув максимумів цих смуг у бік довгих хвиль. Півширина смуги та величина зсуву збільшується у ряду С₆₀—С₆₀ + Pt—С₆₀ + Fe—С₆₀ + Fe + Pt. Разработана методика получения эндо- и экзофуллеренов методом ионной имплантации. Проведены спектрофотометрические исследования растворов малых концентраций полученных металлофуллеренов в органических растворителях. Показано, что присоединение к фуллерену атома металла приводит к увеличению ширины линий в спектре поглощения и смещению максимума поглощения в длинноволновую часть спектра. При этом полуширина и смещение увеличиваются в ряду С₆₀—С₆₀ + Pt—С₆₀ + Fe—С₆₀ + Fe + Pt. en Інститут металофізики ім. Г.В. Курдюмова НАН України Наносистеми, наноматеріали, нанотехнології Obtaining and Spectrophotometric Study of Organic Solutions of C₆₀ Endo- and Exometallofullerenes Article published earlier |
| spellingShingle | Obtaining and Spectrophotometric Study of Organic Solutions of C₆₀ Endo- and Exometallofullerenes Borts, B.V. Tkachenko, V.I. Moskvitin, A.V. Kazarinov, Yu.G. |
| title | Obtaining and Spectrophotometric Study of Organic Solutions of C₆₀ Endo- and Exometallofullerenes |
| title_full | Obtaining and Spectrophotometric Study of Organic Solutions of C₆₀ Endo- and Exometallofullerenes |
| title_fullStr | Obtaining and Spectrophotometric Study of Organic Solutions of C₆₀ Endo- and Exometallofullerenes |
| title_full_unstemmed | Obtaining and Spectrophotometric Study of Organic Solutions of C₆₀ Endo- and Exometallofullerenes |
| title_short | Obtaining and Spectrophotometric Study of Organic Solutions of C₆₀ Endo- and Exometallofullerenes |
| title_sort | obtaining and spectrophotometric study of organic solutions of c₆₀ endo- and exometallofullerenes |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/72477 |
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