Синтез вуглецевих наноструктур при використанні дешевих марок графіту
In the work, carbon nanostructures (CNS) were synthesized on a plasma chemical plant using graphite electrodes SIGE (Special Impregnated Graphite Electrodes) and FGDG-7 (Fine-grained dense graphite) in a helium environment. In the experiments, it was established that graphite electrodes of the SIGE...
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| Date: | 2022 |
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Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine
2022
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| author | Золотаренко, Ол. Д. Рудакова, О. П. Аханова, Н. Е. Уалханова, М. Золотаренко, Ан. Д. Щур, Д. В. Габдуллин, М. Т. Гаврилюк, Н. А. Мироненко, Т. В. Золотаренко, О. Д. Чимбай, М. В. Загорулько, І. В. Тарасенко, Ю. О. Гаврилюк, О. О. |
| author_facet | Золотаренко, Ол. Д. Рудакова, О. П. Аханова, Н. Е. Уалханова, М. Золотаренко, Ан. Д. Щур, Д. В. Габдуллин, М. Т. Гаврилюк, Н. А. Мироненко, Т. В. Золотаренко, О. Д. Чимбай, М. В. Загорулько, І. В. Тарасенко, Ю. О. Гаврилюк, О. О. |
| author_institution_txt_mv | [
{
"author": "Ол. Д. Золотаренко",
"institution": "Інститут хімії поверхні ім. О.О.Чуйка Національної академії наук України \/ Інститут проблем матеріалознавства ім. І.М. Францевича НАН України"
},
{
"author": "О. П. Рудакова",
"institution": "Інститут проблем матеріалознавства ім. І.М. Францевича НАН України"
},
{
"author": "Н. Е. Аханова",
"institution": "Казахсько-британський технічний університет (КБТУ) \/ Казахський національний університет ім. Аль-Фарабі"
},
{
"author": "М. Уалханова",
"institution": "Казахський національний університет ім. Аль-Фарабі"
},
{
"author": "Ан. Д. Золотаренко",
"institution": "Інститут хімії поверхні ім. О.О.Чуйка Національної академії наук України \/ Інститут проблем матеріалознавства ім. І.М. Францевича НАН України"
},
{
"author": "Д. В. Щур",
"institution": "Інститут проблем матеріалознавства ім. І.М. Францевича НАН України"
},
{
"author": "М. Т. Габдуллин",
"institution": "Казахсько-британський технічний університет (КБТУ)"
},
{
"author": "Н. А. Гаврилюк",
"institution": "Інститут хімії поверхні ім. О.О.Чуйка Національної академії наук України"
},
{
"author": "Т. В. Мироненко",
"institution": "Інститут проблем матеріалознавства ім. І.М. Францевича НАН України"
},
{
"author": "О. Д. Золотаренко",
"institution": "Інститут проблем матеріалознавства ім. І.М. Францевича НАН України"
},
{
"author": "М. В. Чимбай",
"institution": "Інститут хімії поверхні ім. О.О.Чуйка Національної академії наук України \/ Інститут проблем матеріалознавства ім. І.М. Францевича НАН України"
},
{
"author": "І. В. Загорулько",
"institution": "Інститут металофізики ім. Г.В. Курдюмова НАН України"
},
{
"author": "Ю. О. Тарасенко",
"institution": "Інститут хімії поверхні ім. О.О.Чуйка Національної академії наук України"
},
{
"author": "О. О. Гаврилюк",
"institution": "Інститут хімії поверхні ім. О.О.Чуйка Національної академії наук України"
}
] |
| author_sort | Золотаренко, Ол. Д. |
| baseUrl_str | |
| collection | OJS |
| datestamp_date | 2023-04-20T10:24:32Z |
| description | In the work, carbon nanostructures (CNS) were synthesized on a plasma chemical plant using graphite electrodes SIGE (Special Impregnated Graphite Electrodes) and FGDG-7 (Fine-grained dense graphite) in a helium environment. In the experiments, it was established that graphite electrodes of the SIGE brand are suitable for the synthesis of CNS by the electric arc plasma chemical method. In addition, the experiments indicate that SIGE graphite in electric arc synthesis in a gas environment allows the creation of centimeter composite rods (deposits), where the core consists of graphene sheets rolled into nanotubes that can withstand extremely high temperatures (>4000 K). Studies using scanning microscopy have shown that the synthetic deposit of SIGE graphite can be divided into blocks, which is important for its use in high voltage stations because it is possible to prepare deposits of the required length without mechanical impact and without violating the integrity of its structure.
The structure of the synthesized carbon materials was studied by scanning and transmission electron microscopy and it was shown that carbon nanotubes are formed during the evaporation of SIGE brand graphite even without the use of a catalyst. Experiments have confirmed that the mass yield of wall fullerene-containing carbon black during the evaporation of SIGE grade graphite significantly exceeds the results obtained during the evaporation of FGDG-7 grade graphite electrodes. Such results make SIGE graphite more productive for the synthesis of expensive carbon nanoproducts (fullerenes and fullerene-like structures) by the electric arc method.
It was also recorded that during the synthesis of carbon nanostructures, single-walled carbon nanotubes are formed, which have a positive charge and are deposited in the form of a core on the surface of the cathode electrode under the action of an electromagnetic field. |
| doi_str_mv | 10.15407/Surface.2022.14.113 |
| first_indexed | 2025-09-24T17:25:28Z |
| format | Article |
| fulltext |
Поверхня. 2022. Вип. 14(29). С. 113–131 113
НАНОМАТЕРИАЛЫ И НАНОТЕХНОЛОГИИ
UDC 537:539 doi: 10.15407/Surface.2022.14.113
SYNTHESIS OF CARBON NANOSTRUCTURES
USING CHEAP GRADES OF GRAPHITE
Ol.D. Zolotarenko1,2, E.P. Rudakova1,2, N.Y. Akhanova3,4, M. Ualkhanova4,
An.D. Zolotarenko1,2, D.V. Shchur2, M.T. Gabdullin3, N.A. Gavrylyuk1,
T.V. Myronenko2, A.D. Zolotarenko2, M.V. Chymbai1,2, I.V. Zagorulko5,
Yu.O. Tarasenko1, O.O. Havryliuk1
1 Chuiko Institute of Surface Chemistry, of the N.A.S. of Ukraine, 17General Naumov Str., 03164,
Kyiv, Ukraine, a.d.zolotarenko@gmail.com
2 Frantsevich Institute for Problems of Materials Science of N.A.S. of Ukraine, 3,
Krzhizhanovskogo Str., 03142,Kyiv, Ukraine
3 Kazakhstan-British Technical University, 59, Tole bi Str., 050000, Almaty, Kazakhstan
4 National Nanotechnology Open Laboratory (NNOL), Al-Farabi Kazakh National University, Al-
Farabi, 71, 050040, Almaty, Kazakhstan
5 G.V. Kurdyumov Institute for Metal Physics of the N.A.S. of Ukraine, 36 Academician Vernadsky
Blvd., 03142, Kyiv, Ukraine
In the work, carbon nanostructures (CNS) were synthesized on a plasma chemical plant
using graphite electrodes SIGE (Special Impregnated Graphite Electrodes) and FGDG-7 (Fine-
grained dense graphite) in a helium environment. In the experiments, it was established that
graphite electrodes of the SIGE brand are suitable for the synthesis of CNS by the electric arc
plasma chemical method. In addition, the experiments indicate that SIGE graphite in electric arc
synthesis in a gas environment allows the creation of centimeter composite rods (deposits),
where the core consists of graphene sheets rolled into nanotubes that can withstand extremely
high temperatures (>4000 K). Studies using scanning microscopy have shown that the synthetic
deposit of SIGE graphite can be divided into blocks, which is important for its use in high
voltage stations because it is possible to prepare deposits of the required length without
mechanical impact and without violating the integrity of its structure.
The structure of the synthesized carbon materials was studied by scanning and
transmission electron microscopy and it was shown that carbon nanotubes are formed during the
evaporation of SIGE brand graphite even without the use of a catalyst. Experiments have
confirmed that the mass yield of wall fullerene-containing carbon black during the evaporation
of SIGE grade graphite significantly exceeds the results obtained during the evaporation of
FGDG-7 grade graphite electrodes. Such results make SIGE graphite more productive for the
synthesis of expensive carbon nanoproducts (fullerenes and fullerene-like structures) by the
electric arc method.
It was also recorded that during the synthesis of carbon nanostructures, single-walled
carbon nanotubes are formed, which have a positive charge and are deposited in the form of a
core on the surface of the cathode electrode under the action of an electromagnetic field.
Keywords: nanotechnology, carbon nanostructures (CNS), fullerenes, nanocomposites,
carbon nanotubes (CNT), graphene, deposit, plasma, electric arc synthesis, graphite grade
«Special Impregnated Graphite Electrodes» (SIGE), graphite grade «Fine-grained dense
graphite» (FGDG-7).
114
1. Introduction
The method of electric arc evaporation of graphite in an inert gas environment is relatively
common, productive and quite effective, as allows to obtain both soluble [1 – 11] and insoluble
carbon nanostructures (CNS) [12 – 15]. In 1996, the authors of [16] received the Nobel Prize for
the discovery of fullerenes, and in 2016 the work on the study of soluble carbon nanostructures
(fullerenes) [17] was nominated for the Nobel Prize.
There are other no less perspective methods for the synthesis of carbon nanostructures
[18 – 26], from which it is also possible to create new modern materials [27 – 32]. But only the
electric arc evaporation of the anode can guarantee the synthesis of fullerene molecules in large
quantities. The method allows you to easily change the modes of synthesis, use a gaseous
medium of different chemical composition, and most importantly - to achieve a high percentage
of carbon nanomaterials (CNM) of different chemical composition, structure and morphology.
Such materials can be used to hydrogen store [17, 33 – 36] and compete with existing
materials for hydrogen storages [37 – 65]. The results of such research allow to create modern
technological masterpieces [26, 28, 29, 30, 45, 43, 53, 57, 66 – 69].
For the synthesis of new carbon nanomaterials, FGDG-7 graphite is usually used. The
name of the mark is deciphered as "Fine-grained dense graphite", and the number 7 at the end of
the abbreviation indicates the density of graphite, which is equal to 1700 kg/m3.
The mass production of SIGE graphite brand, which deciphered as "Special Impregnated
Graphite Electrodes", allows it to be used not only in industry, but also to create new production,
based on it. For example, such graphite can be the basis for the synthesis of new carbon
nanomaterials. In addition, the price of SIGE graphite is much lower than the FGDG -7 graphite
brand.
However, for today, the carbon nanoproducts (CNPs)of electric arc synthesis in a gaseous
environment of SIGE graphite brand remains unexplored. Therefore, to use graphite of this brand
in nanotechnology, it is necessary to study and analyze the possibility of carbon nanomaterials
synthesis from it.
The main purpose of this work is realization of comparative studies of products and
technological conditions for the synthesis of carbon nanomaterials from SIGE and FGDG-
7graphite grades.
Such an analysis can reveal a number of advantages of SIGE graphite grade in obtaining of
various CNPs and open the additional opportunities for its use in electric arc synthesis plants.
2. Research methods and equipment
In the process of electric arc synthesis in a gaseous environment, it is possible to evaporate
or spray the anode electrode, which allows you to change the spectrum of synthesized products.
Electrode evaporation is a mode of electric arc synthesis, where the anode component turns
into an atomic state, creating conditions for the СNS synthesis. During this evaporation of the
electrode the fullerenes and fullerene-like structures are synthesized.
Electrode spraying is a mode of electric arc synthesis, where the anode component does
not turn into an atomic state. As a rule, such process takes place at a high feed rate of the cathode
electrode, where the anode does not have time to evaporate, and its graphite component turns
into a deflated state. Our results of studies of this electric arc synthesis mode indicates to the
process of forming graphene packets modified by the used catalyst.
Evaporation mode of the consumable anode electrode was used for the synthesis of CNS
by the electric arc method. The experimental electric arc plasma-chemical synthesis unit consists
of a vertical cylindrical reactor (Fig. 1), in the center of which is a collet (Fig. 1b (3)), which
holds the consumable anode electrode (Fig. 1b (9)). At the above is a collet (Fig. 1b (2)), which
holds a non-consumable cathode electrode (Fig. 1b (7)). In the process of electric arc synthesis
between the electrodes, plasma is generated (Fig. 1b (1)).The consumable anode electrode
115
evaporates in this plasma. The environment of the working chamber of the CNS synthesis reactor
is filled with helium (Fig. 1b (4)).
(а) (b) (c)
Fig. 1. The back view of the electric arc plasma-chemical installation (a), and scheme of the
cylindrical reactor for the CNS synthesis in the gas environment (b): 1 – plasma; 2 – collet,
which holds a non-consumable cathode electrode; 3 – collet for fixing the consumable
anode electrode; 4 – helium containing environment; 5 – wall soot; 6 – deposit; 7 – non-
consumable electrode (cathode); 8 – deposit core; 9 – consumable anode; 10 – catalyst in
the electrodes; 11 – deposit rind; 12 – wall of the reactor, 13 – axis of the reactor for the
CNS synthesis. (c) – schematic representation of rind and core of the approved deposit
Non-expendable cathodes made of high-quality graphite brand FGDG-7, as well as
consumable anode electrodes made of graphite brand SIGE (State Standard ISO 9001-2015) and
graphite brand FGDG -7 (State Standard 26132-84) were used for research.
During the CNS electric arc synthesis, two types of electrodes are used: a consumable
anode electrode (Fig. 1b (9)) and a non-expendable cathode electrode (Fig. 1b (7)). Near the
vertical reactor (Fig. 1) a non-expendable cathode electrode (Fig. 1b (7)) moves bridging of the
reactor axis (Fig. 1b (13)) when evaporating a fixed consumable anode electrode in plasma (Fig.
1b (1)) under a pressure of 0.02-0.09 MPa in the helium environment (Fig. 1b (4)). In this
manner, the equal growth of soot (Fig. 1b (5)) can be ensured from all of the reactor wall, and
the same thermodynamic means for the synthesis of all CNM and condensation can be reached.
An empty graphite anode located along the reactor axis (Fig. 1b (13)) was used to
introduce the catalyst into the electric arc synthesis zone. The placed catalyst was in the form of
116
a wire or powder and it was fixing it in the anode cavity with pressed graphite dust (Fig. 1b
(10)).
Anodes of different geometric sizes were used (0,9×0,9×48 сm; 1,5×1,5×48 сm;
2×2×48 сm; 2,5×2,5×48 сm).
In this work, the study of morphology and structure at the micro- and nanoscale materials
formed by electric arc evaporation in a gaseous environment of graphite grades SIGE and
FGDG-7, and studied the effect of vapors of chemical impurities in graphite (Si, Fe, Al, Mg, Cu,
B, Mn) for the formation of carbon nanostructures, were carried out.
Comparison of the content of some elements - impurities in the graphite grades SIGE
(produced by "Ukrgrafit") and FGDG-7 are given in table 1. Comparisons of other characteristics
of graphite grades SIGE and FGDG-7 are given in table. 2.
Table 1. The content of some elements in graphite gradesFGDG-7 (State Standard 26132-84)
and brand SIGE (State Standard ISO 9001-2015)
Impurities, % Graphite grade SIGE*
Graphite grade
FGDG-7
Silicon (Si) 4,6 ×10-3 ̶
Iron (Fe) 9,0 ×10-2 1 ×10-3
Aluminum (Al) 6,4 ×10-4 1 ×10-3
Magnesium (Mg) 4,1×10-3 ̶
Copper (Cu) 0,14 ×10-4 1 ×10-4
Boron (B) 0,31 ×10-4 3 ×10-4
Manganese (Mn) 0,14×10-4 5 ×10-5
Calcium (Са) 2,4 ×10 -2 ̶
Titanium (Тi) 4,8 ×10 -4 ̶
Sodium (Na) 3,1 ×10 -4 ̶
The total content of impurities, % 0,3 ̶
* the content of only some of the impurities is given.
Table 2. CharacteristicsofgraphitegradesFGDG-7 and SIGE
Characteristic Graphite grade SIGE
Graphite grade
FGDG-7
Density, g/cm3, not less 1,55 1,72
Compressive strength, MPa, not less ̶ 65
Bending strength, MPa, not less 6,5 34
Specific resistance, μOhmꞏm, not more 11 18
Ash content,%, not more 0,2 0,25
3. Research results and discussion
Graphite electrodes of SIGE brand with a size of not more than 0.9 × 0.9 × 48 cm in the
process of evaporation acquired high fragility. Therefore, it was concluded that for the CNS
synthesis it is necessary to evaporate electrodes larger than 0.9 × 0.9 × 48 cm, overall
dimensions. In addition, increasing the cross-sectional area of the consumable electrodes allowed
to increase the quantitative output of fullerene-containing ash in the one synthesis cycle.
117
The duration of arc synthesis of CNS from graphite of SIGE brand was not more than 3
hours with a small overall size of the electrode (0.9×0.9×48 cm), while the evaporation of the
electrode from graphite brand FGDG-7 of the same size lasted in twice as long (6 hours) (Table
3). Also, the evaporation of the graphite electrode of SIGE brand was accompanied by
fluctuations in electric current from 120 to 180 A at a voltage of 14 - 42 V, and evaporation of
the graphite electrode of FGDG-7 brand is accompanied by an electric current of 185 - 200 A at
a voltage of 30 - 33 V (Table 3).In the process of evaporation of SIGE graphite electrodes in the
size of 0.9×0.9×48 cm was calculated that the required power of the electric arc, the average
value of which is 3.98 kW, which is twice less than the evaporation of graphite electrode of
FGDG-7 brand (6.65 kW) (Table 3).
Such difference in the evaporation rates of graphite electrodes of various brands can be
explained by the low density of graphite of SIGE brand (Table 2).
In the process of electric arc synthesis in the gaseous environment on the walls of the
reactor (Fig. 1b (12)) wall soot is formed (Fig. 1b (5)), and on the cathode electrode the deposit
is synthesized (Fig. 1b (6)), which is a by-product of synthesis.
The wall soot is the main product of electric arc synthesis. It contains soluble and insoluble
carbon nanostructures, the nucleation of which occurs in the synthesis zone. Soluble carbon
nanostructures contained in the ash, include fullerenes, endofullerenes and fullerene-like
products. Insoluble carbon nanostructures include carbon nanotubes (CNTs), graphenes and
graphene packets.
The deposit is a by-product of the synthesis formed on the cathode electrode in the form of
an outgrowth, always located along the electrode reactor axis (Fig. 1b (6)). It was found that the
deposit consists of the core and rind of the deposit. Physicochemical studies of the deposit
morphology indicate that the structure of the core and rind of the deposit depends on the catalyst
present in the electric arc synthesis zone.
The deposit core is a component of the deposit formation (Fig. 1b (8)), which has its own
structure and consists of CNTs, which are firmly connected with the rind of the deposit. But it
has been experimentally proven that when using a catalyst in the electric arc synthesis process,
the deposit core is formed as an independent structure in the deposit and it is easily separated
from the rind.
The deposit rind is a component of the deposit formation and is its outer layer (Fig. 1b
(11)). The deposit rind has its own structure and consists of graphene, graphene packaging and
CNTs, which in non-catalytic synthesis are also firmly connected with the core of the deposit.
At the end of the evaporation of the graphite electrode of SIGE brand (0.9×0.9×48 cm), the
mass of the deposit (14 – 16 g) exceeds the mass of fullerene-containing wall soot (6 – 10 g).
Therefore, a mode evaporation of graphite electrode of SIGE brand was developed, in which it is
necessary to spend more power for the electric arc (6.64 kW), and the output of wall soot is more
than 25 grams from one electrode (Table 3). Such high output of near-wall soot in the case of
electric arc evaporation of graphite electrodes of the SIGE brand significantly exceeds the
similar parameter of evaporation of graphite electrodes of the FGDG-7 brand of the same size.
This means that SIGE brand of graphite is a more productive for the synthesis of CNS by
electric-arc method. The general view of the consumable anode electrode after its partial
evaporation is presented in Fig. 2.
Thus, it can be argued that in the process of CNS synthesis during evaporation of the
graphite anode of the SIGE brand, a smaller part of the chemical component forms a deposit, and
the main part of the electrode is spent on the formation of near-wall soot. Wall soot is formed by
moving the active component of the gaseous environment in the zone of lower pressure and
temperature to the periphery until it cools on the reactor wall.
118
(а) (b)
Fig. 2. General view of the consumable anode electrode after its partial evaporation: a) SIGE
graphite brand; b) FGDG-7graphite brand
Table 3. Conditions and results of synthesis of fullerene-containing soot from graphite
electrodes of brands FGDG-7 and SIGE (0.9×0.9×48 cm)
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№4 7.5 40.5 50 45 180 23 0.72 26 21.8 7 2.5 13 17.5 4.5 3:10 4.14
№5 7.5 40.5 53 48 170 42 0.75 25 25 8 2.5 11 19.5 6.5 3:05 7.14
During the synthesis, when the SIGE graphite anode is evaporates, a deposit constantly
formed on the non-consumable cathode electrode (Figs. 3, 4 (a)). It could be formed coaxially
(Fig. 3 (a)) or not coaxially (Fig. 3 (b)) relative to the cathode electrode, but it necessarily
formed coaxially with the consumable anode electrode.
The SIGE graphite deposit also consisted of two parts: a core and a rind, which was
formed by layered graphite-like structures containing a number of multi-walled carbon
119
nanotubes (MCNTs). Schematic representation of the deposit growth in section along its axis is
shown in Fig. 1(c) in the footnote of cross section A-A, which illustrated the rind and core of the
formed deposit.
(а) (b) (c) (d)
Fig. 3. Appearance of SIGE brand graphite deposit (growth on the cathode): (a) - coaxial
cathode deposit; (b) - misaligned cathode deposit; (c) - with carbon nanostructures on the
surface, (d) - the surface of the deposit without carbon nanostructures on the surface
Table. 4. Comparison of conditions and results of synthesis of fullerene-containing soot from
graphite electrodes of brands FGDG-7 and SIGE
C
on
di
tio
ns
Anode material FGDG-7 graphite SIGE graphite
Cathode length, cm 8.4 7.5
Anode length, cm 40.5 40.5
Current strength, A 185 – 200 120 – 180
Voltage, V 30 – 33 14 – 42
Pressure, atm. 0.190 – 0.174 0.70
Reactor cooling jacket temperature, ºC 31 25.6
Synthesis environment Helium Helium
R
es
ul
ts
Soot mass,g 20.4 25
Deposit mass, g 14.5 8
Chips mass, g 9.400 6.5
Anode length after synthesis, cm 4.5 11
Deposit length, cm 5 2.5
Average discharge power, kW 6.65 6.64
Synthesis time, hours 6 3
In compliance with the specially developed evaporation regime of graphite of SIGE brand,
when the maximum amount of fullerene-containing soot synthesizes at an electric arc power of
6.64 kW, and a deposit of 2.5 cm long and 8 g weight is formed. Such characteristics do not
exceed the parameters of the deposit obtained by evaporation of the graphite electrode of FGDG-
7 brand, which had an average length of 5 cm and a weight of 14.5 g (Table 4). At evaporation of
120
the consumable anode electrode of SIGE brand with an average electric arc power of 3.98 kW (at
standard conditions) forms a deposit with a length of 7.8 cm and a weight of 15.95 g. Such
indicators exceed the values of similar parameters of synthesis products from graphite of FGDG-
7 brand (Table 4).
(а) (b) (c)
(d)
Fig. 4. General view of the deposit formed when using SIGE brand graphite: (a) - top view; (b)
side view; (c) - cross section of the deposit, (d) - longitudinal section of the deposit
(section along its axis)
The general view of the deposit formed at using of graphite of the SIGE brand is presented
in fig. 4. The figure shows the form of deposit from above (a), side (b), in cross (c) and
longitudinal (d) sections, where the interfacial boundary between the core and the rind (shell) is
clearly expressed. The main part of the deposit obtained from graphite of SIGE brand, is the core
(Fig. 4 (c, d)), as well as in the deposit of graphite of FGDG-7 brand. Thin crusty shell of the
deposit obtained from SIGE graphite, is rigidly bonded to the core (Fig. 4 c, d).
Upon detailed study of the deposit, you can see that in the synthesis it takes the form of an
anode. That is, if you look at the deposit from above, the core represented a square insert in the
deposit (Fig. 4 (c)). Therefore, if the evaporating anode has a rectangular shape, then the core of
the deposit in the synthesis will acquire a rectangular shape (Fig. 4). This is important for the
creation of a controlled shape composite (carbon nanotubes and graphene packs) in the form of a
deposit out growth that can be resistant to high electrical loads (10 kW) and plasma temperatures
(> 4,000 K).
Analysis of the mechanical strength of the synthesized deposits revealed that the deposit
consists of hemispherical blocks (Fig. 5), enclosed in a single structure, fastened by a shell
(Fig. 4 (d)). Studies have shown that the length of one block of the formed deposit is equal to the
step of feeding the electrode at electric arc synthesis.
The inner (upper) part of the deposit block is visually resembles a hemisphere (Fig. 5 (a)).
It is adjacent to the lower part of the hemispherical block of the deposit, which was formed
121
earlier in the process of electric arc synthesis from SIGE graphite. Separation of deposit blocks is
possible by simple mechanical manipulation.
The lower part of the hemispherical block of the deposit is concave from the anode
electrode to the cathode electrode (Fig. 5 (b)). To visually identify the hemispherical state of the
deposit block at the bottom of its lower part a red paper indicator wasplaced(Fig. 5b). At the
bottom of the formed hemispherical deposit block you can see the formation of a new deposit
block in the process of electric arc synthesis from graphite of the SIGE grade (Fig. 5 (b, c)).
(а) (b) (c)
Fig. 5. Appearance of one of the blocks of SIGE brand graphite deposit: (a) - inner (upper) part
of the hemispherical block; (b) - the lower part of the hemispherical block; (c) is a deposit
block cut along its axis
The phenomenon of the deposit structure, which consists from the blocks, is not observed
in the deposits synthesized from graphite of FGDG-7 grade. Information about the natural
differentiation of the deposit into blocks is important for its use in high voltage blocks. This
allows you to prepare deposits of the required length without mechanical influence and
disruption of its integrality.
According to the results of scanning electron microscopy (SEM) analysis, it was found,
that the shell (rind) of deposits formed by evaporation of graphite electrodes of SIGE and
FGDG-7 brands, consists from layered structures located perpendicular to the deposit axis and
firmly enclosed in a single rigid construction. The results of such studies are shown in Fig. 6.
The deposit core is rigid and monolithic. It consists of graphene sheets rolled into
nanotubes (Fig. 4 (c, d)). When the graphite electrode of the SIGE brand evaporates, a core is
formed. It has the structure of same density as in the deposit obtained from the FGDG-7 graphite
brand.
However, studies of SIGE graphite deposits have shown that its core is very poorly
separated from the deposit shell by mechanical means and cannot exist as a single synthesis
product (rod) without mechanical intervention.
Thus, in the case of electric arc synthesis in a gaseous environment from graphite of the
SIGE brand, it is possible to create centimeter rods resistant to ultra-high temperatures (> 4000 K
[70]).
Due to its layered structure, the deposit shell can be used for graphene obtaining.
Differential thermal (DTA), thermogravimetric (TG) and differential thermogravimetric (DTG)
analyzes showed that the temperature interaction of the deposit shell with air oxygen starts at 575
ºC (Table 5, item 1) and does not exceed the interaction temperature of the deposit core (Table 5,
item 2) (Fig. 9 (a, b)).
122
Fig. 6. Deposition rind for med by layered graphite-like structures (SEM)
The DTA curve (Fig. 7 (b)) indicates the two-phase of core of the deposit obtained by
evaporation of the SIGE brand electrode. This evidences that, in addition to the graphite-like
component, the core contained the multi-walled carbon nanotubes, the growth of which was
initiated by low electric arc power (3.98 kW).
In the process of electric arc synthesis, the CNS is formed on the surface of the deposit of
graphite of SIGE brand(Fig. 3, 4 (a)). According to the results of differential thermal (DTA),
thermogravimetric (TG) and differential thermogravimetric (DTG) analyzes, it was found that
the temperature of the beginning of the interaction of the formed CNS with oxygen is 910 ºC
(Table 5, item 4). This indicates that the deposit surface contains single-walled carbon nanotubes
(SCNT). The data are given in Table. 5, item 4.
(a) (b)
Fig.7. Heat resistance of the deposit obtained by evaporation of the electrode of SIGE brand: (a)
– the shell of the deposit; (b) - the ore of the deposit
That is, in the process of electric arc synthesis of carbon nanostructures, the carbon
nanotubes are formed, which have a positive charge and under the action of an electromagnetic
field are deposited on the surface of the cathode non-consumable electrode in the form of a
deposit (Fig. 3, 4 (a)).
By the method of transmission electron microscopy (TEM) it was found that the core of
the deposit obtained by evaporation of the graphite anode electrode of SIGE brand, consists of
multi-walled carbon nanotubes (MCNT) (Fig. 8).
That is, in the process of electric arc evaporation of the SIGE brand electrode, the non-
catalytic carbon nanotubes (CNTs) are formed. Obtaining CNTs without the use of a catalyst can
reduce their cost.
123
Table 5. Heat resistance of the deposit parts after evaporation by electric arc synthesis in a
gaseous environment of graphite electrode of SIGE brand
s/n
№
Material
Interaction
interval, ºС
DTG DTA
Т1max, ºС Т1max, ºС Т2max, ºС
1 Deposit shell 575 – 980 840 840 -
2 Deposit core 575 – 990 870 850 960
3 Wall soot 575 – 990 800 800 910
4 CNT 575 – 650 650 550 650
Fig. 8. Multiwall carbon nanotubes that are components of the core of the deposit obtained by
evaporation of the graphite anode electrode of SIGE brand (TEM)
Fig. 9. The surface of the wall soot of the graphite electrode of SIGE brand at tersonication in
ethyl alcohol (SEM)
Fig. 10. Wall soot, which contains carbon nanosized particles (TEM)
124
Fig. 11. Express analysis of the content of the
soluble component of soot fractions C60
and C70: (a) - does not confirm the
presence of fullerenes C60 and C70 in the
first three samples (Table 3, item 1,2,3);
(b) - confirms the presence of fullerenes
C60 and C70 in the last two samples
(Table 3, item 4,5)
(а) (b)
The condensate mixture of the graphite electrode vapor of the SIGE brand is formed in the
gas phase, forming a near-wall soot. It contains both soluble and insoluble components of the
fraction. The insoluble fraction of wall soot includes CNTs and similar structures.
The structure of the wall soot layer at the micro level was determined by scanning electron
microscopy (Fig. 9). Layers of wall soot were previously sonicated in alcohol. Carbon
nanostructures that are part of the wall soot have different geometric shapes and structures
(Fig. 10).
Thermal analysis of near-wall soot synthesized from SIGE graphite showed that there are
two phases that react with oxygen at temperatures of 800 ºC and 910 ºC (Table 4, item 3), as well
as in wall soot obtained at evaporation of the graphite electrode of graphite brand FGDG-7.
Wall soot also contains a soluble component fraction in liquid hydrocarbons. The soluble
fraction contains fullerene-like products and hydrocarbon clusters, fuel oils and other
components.
Using express analysis, we established that the wall soot obtained from the graphite
consumable anode electrode of the FGDG brand (0.9×0.9×48 cm) also contains the soluble
component fraction C60 and C70 (Fig. 11) in the last two samples from five (Table 3, items 4, 5).
Therefore, fullerenes and fullerene-like products were not formed in the first three samples of
wall soot (Table 3, items 1, 2, 3) due to the low power of the electric arc (3.98 kW). Thus, it is
necessary to withstand the electric current power of 6.64 kW for the formation of fullerenes and
fullerene-like nanoproducts from SIGE graphite, which does not exceed the synthesis parameters
during evaporation of FGDG-7 graphite.
The soluble constituent fraction of wall soot can be determined spectrophotometrically.
This method allows not only to identify fullerenes C60 and C70, but also to show the presence of
higher and lower fullerenes in soot. This method of analysis confirmed the presence of fullerenes
C60 and C70 in fullerene-containing soot (Table 3, items 4,5), obtained by different modes of
electric arc synthesis in the process of evaporation of the graphite electrode of SIGE brand
(Fig. 11-12).
Calculations based on photospectral analysis data showed that the fullerene component in
the obtained two samples of soot (Table 3, items 4, 5) from graphite of SIGE brand, contains
from 10% to 12% of fullerenes. This content exceeds the concentration of the fullerene
component in the soot obtained by electric arc evaporation of the graphite electrode of FGDG-
7grade.
125
Fig. 12. Optical density UF-Vis spectroscopy, which detects the presence of C60 and C70 in
solutions of wall soot of two samples (Table 3, items 4,5): (a) - the spectrum of a
solution of fullerene-containing soot of the 4th sample (Table 3, item 4); (b) - the
spectrum of a solution of fullerene-containing soot of the 5th sample (Table 3, item 5)
In addition, the calculations according to photospectral analysis data confirmed the
presence of fullerenes C60 and C70 in a ratio of 74:25% in 2 samples of wall soot extract (Table 3,
items 4,5), obtained from graphite of SIGE brand.
4. Conclusions
Studies have shown that graphite electrodes of SIGE brand are suitable for the synthesis of
carbon nanomaterials by electric arc method in a gaseous environment.
It has been experimentally proven that SIGE graphite in electric arc synthesis in gaseous
environmental lows to create centimeter composite rods (deposits), the core of which consists of
graphene sheets rolled into nanotubes that can withstand ultra-high temperatures (> 4000 K). This
product is very important for creating high voltage equipment.
Scanning microscopy studies have shown that the deposit synthesized from SIGE graphite,
can be divided into blocks, which is important for its use in high voltage stations because it is
possible to prepare deposits of the required length without mechanical impact and without
contravention the integrity of its construction.
Transmission electron microscopy studies have shown that non-catalytic carbon nanotubes
(CNTs) are formed during the electric arc evaporation of the SIGE graphite electrode. Obtaining
CNTs without the use of a catalyst can reduce their cost.
Itis shown that the overall magnification in the consumable anode electrode allows to
increase the quantitative output of fullerene-containing soot.
Experimental studies have confirmed that the output by weight of near-wall fullerene-
containing soot by evaporation of SIGE graphite significantly exceeds the results obtained by
evaporation of FGDG-7 graphite electrodes. These results make SIGE graphite more productive
for the synthesis of expensive carbon nanoproducts (fullerenes and fullerene-like structures) by
the electric arc method.
It is determined that in the process of synthesis of carbon nanostructures the single-walled
carbon nanotubes are formed. They have a positive charge and are deposited in the form of a core
on the cathode electrode surface under the action of an electromagnetic field.
Today, the single-walled carbon nanotubes (SCNTs) are the most expensive type of carbon
nanotubes, and non-catalytic synthesis of SCNTs significantly reduces their cost.
Calculation and experimental results showed that the fullerene component in the two
obtained samples of fullerene-containing soot from graphite of SIGE brand is from 10 to 12 wt.
%, which is not worse, and sometimes better than FGDG-7 graphite.
126
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СИНТЕЗ ВУГЛЕЦЕВИХ НАНОСТРУКТУР
ПРИ ВИКОРИСТАННІ ДЕШЕВИХ МАРОК ГРАФІТУ
Ол.Д. Золотаренко1,2, О.П. Рудакова1,2, Н.Е. Аханова3,4, М. Уалханова4,
Ан.Д. Золотаренко1,2, Д.В. Щур2, М.Т. Габдуллин3, Н.А. Гаврилюк1,
Т.В. Мироненко2, О.Д. Золотаренко2, М.В. Чимбай1,2, І.В. Загорулько5,
Ю.О. Тарасенко1, О.О. Гаврилюк1
1Інститут хімії поверхні ім. О.О. Чуйка НАН України, вул. Генерала Наумова, 17,
03164 Київ, Україна, a.d.zolotarenko@gmail.com
2Інститут проблем матеріалознавства ім. І.М. Францевича НАН України, вул.
Кржижановського, 3, 03142 Київ, Україна
3Казахсько-британський технічний університет (КБТУ), Толі бі 59, пр. Аль-Фарабі,
050040 Алмати, Казахстан
4Національна нанотехнологічна лабораторія відкритого типу (NNLOT), Казахський
національний університет ім. Аль-Фарабі, д. 71, пр. Аль-Фарабі,
050040 Алмати, Казахстан
5Інститут металофізики ім. Г.В. Курдюмова НАН України, бульв. Акад. Вернадського, 36,
03142 Київ, Україна
131
У роботі синтезовані вуглецеві наноструктури (ВНС) на плазмохімічній установці
при використанні графітових електродів ЕГСП (Спеціально імпрегновані графітові
електроди) та МПГ-7 (Дрібно зернистий щільний графіт) в середовищі гелію. В
експериментах встановлено, що графітові електроди марки ЕГСП придатні для синтезу
ВНС електродуговим плазмохімічним методом. Крім того, експерименти вказують на
те, що графіт марки ЕГСП в електродуговому синтезі в газовому середовищі дозволяє
створити сантиметрові композитні стрижні (депозити), де серцевина складається з
графенових листів, згорнутих в нанотрубки, які витримують надвисокі температури
(>4000 К). Дослідження за допомогою скануючої мікроскопії показали, що синтезований
депозит з графіту марки ЕГСП може розділятися на блоки, що важливо для його
використання в станціях високого напруження тому, що можна готувати депозити
необхідної довжини без механічного впливу і не порушуючи цілісність його конструкції.
Дослідження за допомогою просвітлюванної мікроскопії показали, що в процесі
електродугового випаровування електрода марки ЕГСП формуються безкаталітичні
вуглецеві нанотрубки). Експерименти підтвердили, що вихід по масі пристінної
фуллеренвмісної сажі при випаровуванні графіту марки ЕГСП значно перевищує
результати, отримані при випаровуванні графітових електродів марки МПГ-7. Такі
результати роблять графіт марки ЕГСП більш продуктивним для синтезу дорогих
вуглецевих нанопродуктів (фуллеренів та фуллереноподібних структур) електродуговим
методом.
Також зафіксовано, що в процесі синтезу вуглецевих наноструктур формуються
одностінні вуглецеві нанотрубки, які мають позитивний заряд і під дією
електромагнітного поля осаджуються у вигляді серцевини на поверхні катодного
електрода.
Ключові слова: нанотехнології, вуглецеві наноструктури (ВНС), фуллерени,
нанокомпозити, вуглецеві нанотрубки (ВНТ), графен, осадження, плазма, електродуговий
синтез, графіт марки (SIGE) «Спеціально імпрегновані графітові електроди», графіт
марки (FGDG-7) «Дрібно зернистий щільний графіт».
|
| id | oai:ojs.pkp.sfu.ca:article-750 |
| institution | Surface |
| keywords_txt_mv | keywords |
| language | English |
| last_indexed | 2025-09-24T17:45:58Z |
| publishDate | 2022 |
| publisher | Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine |
| record_format | ojs |
| resource_txt_mv | surfacezbircomua/d7/8938a3e842ab6238c4264858a744b5d7.pdf |
| spelling | oai:ojs.pkp.sfu.ca:article-7502023-04-20T10:24:32Z Synthesis of carbon nanostructures using cheap grades of graphite Синтез вуглецевих наноструктур при використанні дешевих марок графіту Золотаренко, Ол. Д. Рудакова, О. П. Аханова, Н. Е. Уалханова, М. Золотаренко, Ан. Д. Щур, Д. В. Габдуллин, М. Т. Гаврилюк, Н. А. Мироненко, Т. В. Золотаренко, О. Д. Чимбай, М. В. Загорулько, І. В. Тарасенко, Ю. О. Гаврилюк, О. О. nanotechnology carbon nanostructures (CNS) fullerenes nanocomposites carbon nanotubes (CNT) graphene deposit plasma electric arc synthesis graphite grade «Special Impregnated Graphite Electrodes» (SIGE) graphite grade «Fine-grained dense graphite» (FGDG-7) нанотехнології вуглецеві наноструктури (ВНС) фуллерени нанокомпозити вуглецеві нанотрубки (ВНТ) графен осадження плазма електродуговий синтез , графіт марки (SIGE) «Спеціально імпрегновані графітові електроди» графіт марки (FGDG-7) «Дрібно зернистий щільний графіт» In the work, carbon nanostructures (CNS) were synthesized on a plasma chemical plant using graphite electrodes SIGE (Special Impregnated Graphite Electrodes) and FGDG-7 (Fine-grained dense graphite) in a helium environment. In the experiments, it was established that graphite electrodes of the SIGE brand are suitable for the synthesis of CNS by the electric arc plasma chemical method. In addition, the experiments indicate that SIGE graphite in electric arc synthesis in a gas environment allows the creation of centimeter composite rods (deposits), where the core consists of graphene sheets rolled into nanotubes that can withstand extremely high temperatures (>4000 K). Studies using scanning microscopy have shown that the synthetic deposit of SIGE graphite can be divided into blocks, which is important for its use in high voltage stations because it is possible to prepare deposits of the required length without mechanical impact and without violating the integrity of its structure. The structure of the synthesized carbon materials was studied by scanning and transmission electron microscopy and it was shown that carbon nanotubes are formed during the evaporation of SIGE brand graphite even without the use of a catalyst. Experiments have confirmed that the mass yield of wall fullerene-containing carbon black during the evaporation of SIGE grade graphite significantly exceeds the results obtained during the evaporation of FGDG-7 grade graphite electrodes. Such results make SIGE graphite more productive for the synthesis of expensive carbon nanoproducts (fullerenes and fullerene-like structures) by the electric arc method. It was also recorded that during the synthesis of carbon nanostructures, single-walled carbon nanotubes are formed, which have a positive charge and are deposited in the form of a core on the surface of the cathode electrode under the action of an electromagnetic field. У роботі синтезовані вуглецеві наноструктури (ВНС) на плазмохімічній установці при використанні графітових електродів ЕГСП (Спеціально імпрегновані графітові електроди) та МПГ-7 (Дрібно зернистий щільний графіт) в середовищі гелію. В експериментах встановлено, що графітові електроди марки ЕГСП придатні для синтезу ВНС електродуговим плазмохімічним методом. Крім того, експерименти вказують на те, що графіт марки ЕГСП в електродуговому синтезі в газовому середовищі дозволяє створити сантиметрові композитні стрижні (депозити), де  серцевина складається з графенових листів, згорнутих в нанотрубки, які витримують надвисокі температури (>4000 К). Дослідження за допомогою скануючої мікроскопії показали, що синтезований депозит з графіту марки ЕГСП може розділятися на блоки, що важливо для його використання в станціях високого напруження тому, що можна готувати депозити необхідної довжини без механічного впливу і не порушуючи цілісність його конструкції. Дослідження за допомогою просвітлюванної мікроскопії показали, що в процесі електродугового випаровування електрода марки ЕГСП формуються безкаталітичні вуглецеві нанотрубки). Експерименти підтвердили, що вихід по масі пристінної фуллеренвмісної сажі при випаровуванні графіту марки ЕГСП значно перевищує результати, отримані при випаровуванні графітових електродів марки МПГ-7. Такі результати роблять графіт марки ЕГСП більш продуктивним для синтезу дорогих вуглецевих нанопродуктів (фуллеренів та фуллереноподібних структур) електродуговим методом. Також зафіксовано, що в процесі синтезу вуглецевих наноструктур формуються одностінні вуглецеві нанотрубки, які мають позитивний заряд і під дією електромагнітного поля осаджуються у вигляді серцевини на поверхні катодного електрода. Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine 2022-11-30 Article Article application/pdf https://surfacezbir.com.ua/index.php/surface/article/view/750 10.15407/Surface.2022.14.113 Surface; No. 14(29) (2022): Surface; 113-131 Поверхность; № 14(29) (2022): Поверхня; 113-131 Поверхня; № 14(29) (2022): Поверхня; 113-131 3154-8091 3154-8083 10.15407/Surface.2022.14 en https://surfacezbir.com.ua/index.php/surface/article/view/750/744 Авторське право (c) 2022 Ол.Д. Золотаренко, О.П. Рудакова, Н.Е. Аханова, М. Уалханова, Ан.Д. Золотаренко, Д.В. Щур, М.Т. Габдуллин, Н.А. Гаврилюк, Т.В. Мироненко, О.Д. Золотаренко, М.В. Чимбай, І.В. Загорулько, Ю.О. Тарасенко, О.О. Гаврилюк |
| spellingShingle | нанотехнології вуглецеві наноструктури (ВНС) фуллерени нанокомпозити вуглецеві нанотрубки (ВНТ) графен осадження плазма електродуговий синтез графіт марки (SIGE) «Спеціально імпрегновані графітові електроди» графіт марки (FGDG-7) «Дрібно зернистий щільний графіт» Золотаренко, Ол. Д. Рудакова, О. П. Аханова, Н. Е. Уалханова, М. Золотаренко, Ан. Д. Щур, Д. В. Габдуллин, М. Т. Гаврилюк, Н. А. Мироненко, Т. В. Золотаренко, О. Д. Чимбай, М. В. Загорулько, І. В. Тарасенко, Ю. О. Гаврилюк, О. О. Синтез вуглецевих наноструктур при використанні дешевих марок графіту |
| title | Синтез вуглецевих наноструктур при використанні дешевих марок графіту |
| title_alt | Synthesis of carbon nanostructures using cheap grades of graphite |
| title_full | Синтез вуглецевих наноструктур при використанні дешевих марок графіту |
| title_fullStr | Синтез вуглецевих наноструктур при використанні дешевих марок графіту |
| title_full_unstemmed | Синтез вуглецевих наноструктур при використанні дешевих марок графіту |
| title_short | Синтез вуглецевих наноструктур при використанні дешевих марок графіту |
| title_sort | синтез вуглецевих наноструктур при використанні дешевих марок графіту |
| topic | нанотехнології вуглецеві наноструктури (ВНС) фуллерени нанокомпозити вуглецеві нанотрубки (ВНТ) графен осадження плазма електродуговий синтез графіт марки (SIGE) «Спеціально імпрегновані графітові електроди» графіт марки (FGDG-7) «Дрібно зернистий щільний графіт» |
| topic_facet | nanotechnology carbon nanostructures (CNS) fullerenes nanocomposites carbon nanotubes (CNT) graphene deposit plasma electric arc synthesis graphite grade «Special Impregnated Graphite Electrodes» (SIGE) graphite grade «Fine-grained dense graphite» (FGDG-7) нанотехнології вуглецеві наноструктури (ВНС) фуллерени нанокомпозити вуглецеві нанотрубки (ВНТ) графен осадження плазма електродуговий синтез графіт марки (SIGE) «Спеціально імпрегновані графітові електроди» графіт марки (FGDG-7) «Дрібно зернистий щільний графіт» |
| url | https://surfacezbir.com.ua/index.php/surface/article/view/750 |
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