Дослідження частинок на поверхні Ni-Fe каталізаторів гідрогенування СО2 методом ТД МС аналізу
The condition of Ni-Fe catalysts’ surface was investigated by the method of thermally programmed desorption with mass spectral analysis of desorbed particles (TD MS). TD spectra indicated the desorption of CO2 (m/z = 44), CO (m/z = 28) and H2O (m/z = 18) particles from the surface of samples with hi...
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Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine
2017
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Surface| _version_ | 1869291796436090880 |
|---|---|
| author | Meshkini Far, R. Dyachenko, A. Bieda, O. Ischenko, O. |
| author_facet | Meshkini Far, R. Dyachenko, A. Bieda, O. Ischenko, O. |
| author_institution_txt_mv | [
{
"author": "R. Meshkini Far",
"institution": "Київський національний університет імені Тараса Шевченка"
},
{
"author": "A. Dyachenko",
"institution": "Київський національний університет імені Тараса Шевченка"
},
{
"author": "O. Bieda",
"institution": "Київський національний університет імені Тараса Шевченка"
},
{
"author": "O. Ischenko",
"institution": "Київський національний університет імені Тараса Шевченка"
}
] |
| author_sort | Meshkini Far, R. |
| baseUrl_str | |
| collection | OJS |
| datestamp_date | 2018-12-01T11:32:03Z |
| description | The condition of Ni-Fe catalysts’ surface was investigated by the method of thermally programmed desorption with mass spectral analysis of desorbed particles (TD MS). TD spectra indicated the desorption of CO2 (m/z = 44), CO (m/z = 28) and H2O (m/z = 18) particles from the surface of samples with high and low catalytic activity in the reaction of CO2 hydrogenation. Intermediate compounds CHO*, CH2O* were not observed in the TD profiles for all investigated catalysts. On the basis of catalytic performance results and thermal desorption data it can be suggested that process of CO2 hydrogenation over Ni-Fe catalysts proceeds via direct hydrogenation of CO2 to CH4. |
| doi_str_mv | 10.15407/Surface.2017.09.104 |
| first_indexed | 2025-09-24T17:25:25Z |
| format | Article |
| fulltext |
Поверхность. 2017. Вып. 9(24). С. 104–110 104
PACS/topics 82.30.Hk, 82.30.-b, 82.20.-w
SURFACE SPECIES INVESTIGATION OF Ni-Fe CATALYSTS
OF CO2 HYDROGENATION BY TD MS ANALYSIS
R. Meshkini Far, A. Dyachenko, O. Bieda, O. Ischenko
Taras Shevchenko Kyiv National University Volodymyrska str., 64, Kyiv, 01601, Ukraine
r.meshkinifar@gmail.com
The condition of Ni-Fe catalysts’ surface was investigated by the method of thermally
programmed desorption with mass spectral analysis of desorbed particles (TD MS). TD spectra
indicated the desorption of CO2 (m/z = 44), CO (m/z = 28) and H2O (m/z = 18) particles from the
surface of samples with high and low catalytic activity in the reaction of CO2 hydrogenation.
Intermediate compounds CHO*, CH2O
* were not observed in the TD profiles for all investigated
catalysts. On the basis of catalytic performance results and thermal desorption data it can be
suggested that process of CO2 hydrogenation over Ni-Fe catalysts proceeds via direct
hydrogenation of CO2 to CH4.
Keywords: Ni-Fe catalysts; CO2 hydrogenation; catalytic activity; TD-MS analysis.
Introduction
Carbon dioxide is a component widely existing in nature, but is regarded as an air pollutant,
so it’s needed to reduce the concentration of it in the nature. One of the obvious ways is to reduce
pollution by CO2 by means of the catalytic conversion of waste CO2 emitted from, i.e., enterprise.
Among of various methods, hydrogenation of carbon dioxide not only reduces carbon dioxide but
also produces methane. Methane is the cleanest fossil fuel for electricity production [1 – 3].
Therefore, developing a catalyst that can improve activity, selectivity, economic and
environmental requirements to industrialize the process for carbon dioxide hydrogenation is very
important. Carbon dioxide molecule is kinetically and thermodynamically stable so the reaction
of carbon dioxide hydrogenation is endothermic and calls for use of efficient catalysts to obtain
high methane yield. This reaction has been studied over metal catalysts Ni, Fe, Co, Cu, Ru, and
Rh that were supported on SiO2, Al2O3, ZrO2, TiO2, and CeO2 metal oxides [3 – 7]. According to
the literature, among these catalysts, the iron unlike the nickel has low activity in catalysis of the
hydrogenation of CO2 [8, 9], although a computational screening study based on density
functional theory calculations has indicated that Ni-Fe catalysts could be more active than the
pure Ni catalyst [10]. So, the catalytic properties of bimetallic Ni-Fe catalyst seem to be
promising for using in environmentally safe process.
It is important to study the surface properties of Ni-Fe system for understanding of
mechanism for CO2 hydrogenation. In the previous work we investigated catalytic structure and
showed the efficiency of using Ni-Fe catalysts in the CO2 hydrogenation [11, 12]. In this work,
surface species adsorption properties of Ni-Fe catalysts of CO2 hydrogenation with different
Ni:Fe ratio were investigated by TD MS analysis.
Experimental
Synthesis of Ni-Fe catalysts in the range of 0 – 100 mass % of nickel, with respective addition
of iron was carried out by dissolving the proper amount of metals in nitric acid with subsequent
105
precipitation by ammonia and drying in air for 4 hours at 300 °C. Prior to the catalytic reaction,
each catalyst was reduced with a mixed stream of hydrogen and helium at a ratio of 50:50 vol. %
at 300 °C for 4 hours. The optimal temperature for catalysts reduction was determined with
thermogravimetric method [11].
Methane production test for bimetallic Ni-Fe catalysts was carried out in a continuous flow
fixed-bed reactor with 8 mm in diameter. Carbon dioxide and hydrogen were continuously fed
into the reactor balanced with helium. Feed composition was fixed at 2 vol. % of CO2, 55 vol. %
of H2 and 43 vol. % of He. The reaction was carried out at the pressure of 0,1 MPa in the
temperature range of 30 – 500 °C. Reaction products were analyzed by an online gas
chromatograph (Shimadzu GC-2014) equipped with a thermal conductivity detector (TCD) using
a molecular sieves packed column for the separation of CO2, CO, CH4. To compare the catalytic
activities for the series, we chose the temperature of 350 °C at which the most active samples
reached a steady maximum of activity.
To study the desorbed particles from the surface of the catalyst a quadrupole mass
spectrometer (MS) MX 7304 (“Selmi”, Ukraine) was used. The reduced catalyst was exposed
under hydrogenation experiment conditions. The catalyst then was cooled to ambient
temperature, and then heated linearly in vacuum at 14°/min up to 800 °C while the effluent
stream was analyzed for m/z range of 10 – 100 by on-line MS МХ7304А.
Results and discussion
In the first part of our research, the catalytic behavior of bimetallic Ni-Fe catalysts in the range
of concentrations from 0 to 100 % of nickel was studied [11]. The chemical composition and the
results of the catalytic performance tests of the Ni-Fe catalysts under investigation are
summarized in Table 1. Based on the results, the higher yield of CH4 is observed at the
temperature of 300–400 °C and it drops sharply at the temperature of 500 °C. The maximum CH4
yields reaching 66.5 % were obtained at 350 °C for Ni80Fe20 catalyst.
Table 1. The chemical composition and the results of catalytic performance test of Ni-Fe
catalysts in the reaction of CO2 hydrogenation
Sample Yield, % Sample Yield, %
mass % Temperature, °C mass % Temperature, °C
Ni Fe
Reaction
product
300 350 400 500 Ni Fe
Reaction
product
300 350 400 500
CH4 32 53.8 60.1 5.2 CH4 50.8 62 59.1 2
100 0
CO 3.8 7 8.5 5
70 30
CO 6.2 4.1 4.9 5
CH4 65.8 65 60.4 7.9 CH4 27.8 40 41.4 7.4
90 10
CO 1.3 1.4 1.4 1.3
50 50
CO 2.3 2.6 3.9 2.4
CH4 65.8 66.5 61.9 9.9 CH4 15 35 15 4.5
80 20
CO 2 1.5 1.5 1.5
20 80
CO 2.2 2.5 4.5 2.3
CH4 6.4 15 1.1 2.1 CH4 0 0 1.5 6.6
75 25
CO 10.9 18 9.1 1.3
0 100
CO 10.8 36.4 34.8 4.2
Apart from methane, carbon monoxide is observed as a reaction product in all cases.
However, a CO production increase is associated with a methane production decrease. The
highest yield of CH4 was observed for the sample with 80 mass. % of Ni (Ni80Fe20), whereas for
the sample with 75 mass. % of Ni (Ni75Fe25) catalytic performance drops sharply and reaches a
relative minimum in CO2 hydrogenation. While all other catalysts always show higher selectivity
106
to CH4 than to CO, Ni75Fe25 catalyst gives rise to higher selectivity for CO than for CH4.
According to the studies of Fe-Ni alloys [13], when nickel content is in a concentration range of
less than 72 % or more than 77 %, two-phase regions with γ-phase and intermetallic FeNi3 are
observed. But in the composition range 72–77 % of nickel, there is only FeNi3 compound in the
form of a homogeneous solid solution [13].
The observed effect of the catalytic activity increase (increase of methane yield at the
same conditions) in the Ni80Fe20 sample is related to the presence of phase interfaces in the
catalytic systems. It is known that the catalytic activity of mixtures depends on the phase
composition. The heterogeneous mixtures have higher catalytic activity then homogeneous phase
due to interface properties. Moreover, the catalytic properties of the mixtures depend on the
presence of the organized structures and chemical compounds in them. The formation of
intermetallic compounds reduces the catalytic activity of the system [14].
Among the studied samples we have selected pure nickel, pure iron, the best (Ni80Fe20)
and the worst (Ni75Fe25) catalysts. Desorption of particles from the surface active site of these
samples was investigated by TD MS analysis. For Ni80Fe20, Ni75Fe25 and Ni samples methane and
carbon monoxide are the products of hydrogenation process, while in the case of pure Fe sample
methane is not formed at all, and the only carbon monoxide is product of CO2 and Н2 interaction.
The experimental data shows that the desorption peaks of CO, CO2 and H2O are
symmetrical (Fig.). It suggests that CO, CO2, and H2O molecules are formed near the surface by
recombination of the corresponding atoms. It means that the carbon, oxygen and hydrogen atoms
exist separately on the catalyst surface [15]. Generally, if a process undergoes a formal kinetics
nk
dt
d
,
where is surface coverage and n is the kinetic order of the process, in the case of linear heating
the peak (rate versus temperature) must be asymmetrical for n = 1 and nearly symmetrical for
n = 2 [15]. The symmetrical form of all desorption peaks, even for CO, suggests the second order
of desorption, thus, the recombination of separate atoms into the CO molecule.
TD data of the maximum peak temperature (Tm) can be divided into three ranges (see Table
2): 80–180°С – particles weakly bound to the surface; 200 – 350°С – particles with desorption
temperature close to reaction of hydrogenation temperature; 400–500°С – particles firmly bound
to catalyst surface.
Table 2. The peaks temperature (Tm) of desorbed particles from the samples’ surface
Particle
Sample
СO (m/z = 28) CO2 (m/z = 44) H2O (m/z = 18)
Ni80Fe20 100, 140, 290, 440 90, 145, 300, 440 90, 210
Ni75Fe25 300 300 90, 210
Ni 245, 300, 440 100, 150, 240, 300 90, 175, 230
Fe 100, 260, 440 100, 270, 440 90
107
100 200 300 400 500 600
0
10
20
30
T, 0C
1
2
3
4
a
I, r.u.
100 200 300 400 500 600
0
10
20
30
40
T, 0C
43
1
2
b
I, r.u.
0 100 200 300 400 500 600
15
30
45
60
T, 0C
2
1
4
3
c
I, r.u.
Fig. TD profile of CO (a), CO2 (b) and H2O (c) particles for the samples: 1 – Ni80Fe20,
2 – Ni75Fe25, 3 – Ni and 4 – Fe.
TD spectra of CO and CO2 from surface of Ni75Fe25 catalyst has the only maximum at
300 °C, but for surface of Ni80Fe20 there are peaks in the range of 90–440 °C. TD maximum at
130°C can be attributed to the weak physical adsorption.
TD spectra of CO from surface of inactive Ni75Fe25 catalyst has the greater intensity than
for CO2, in good agreement with the results of the catalytic performance (Table 1) which show
that between all of the tested catalysts the lowest yield of CH4 (6 %) and the highest yield of CO
(11 %) at 300 °C (see Table 1) are observed for Ni75Fe25 catalyst. Thus, it can be assumed that
CO2, which is adsorbed on the active site, breaks up into CO and O. CO is firmly chemisorbed on
the active site and inhibits the progress of CO2 hydrogenation process. In contrast, the intensity of
the TD spectra of CO2 and CO from surface of active Ni80Fe20 catalyst is almost the same at
300°C. Based on these results, we can conclude that process of CO2 hydrogenation over Ni-Fe
catalysts proceeds via direct hydrogenation of CO2 to CH4. The chemisorbed CO2 on the catalyst
active centers, which are located at the interface boundary, is dissociated completely to C*
ads and
O*
ads. Then adsorbed carbon quickly reacts with available hydrogen (adsorbed on the catalysts
surface or from the gas phase) and CH4 is desorbed in result. Water is formed by the similar
mechanism from the adsorbed oxygen and available hydrogen. The limiting step in this process is
the formation of H2O from the adsorbed OH*
ads group with adsorbed H*
ads. The formation of CH4
is fast, so in the TD spectra CH*, CH2
*, CH3
* intermediates are not recorded. TD MS analysis of
surface species in active and inactive samples showed that CO2 hydrogenation process onto Ni–
Fe catalysts has the mechanism that does not involve oxygen-containing intermediates. If the
108
process proceeds via an intermediate CO, the TD spectra of intermediates, namely CHO*, CH2O
*
would have been recorded. The data shown in Fig. 1c indicate that there is no peak of water on
the TD spectrum from surfaces of Ni80Fe20 and Ni75Fe25 at 300 °C, and this fact confirms that the
oxygen is generated by dissociation of CO2 rather than by dissociation of water at this
temperature. These results are in good agreement with the mechanism that was reported in the
previous literature [16].
From the results of catalytic performance and thermal desorption one can suggest the
following mechanism for the reaction of CO2 hydrogenation over Ni-Fe catalysts:
1. СО2 + [ ] → [О…..С…..О]
2. [О…..С…..О] → [С] + 2[О]
3. Н2 +2 [ ] → 2[Н]
4. [С] + [Н] → [СН] + [ ]
5. [СН] + [Н] → [СН2] + [ ]
6. [СН2] + [Н] → [СН3] + [ ]
7. [СН3] + [Н] → СН4 + 2[ ]
8. [О] + [Н] → [ОН] + [ ]
9. [ОН] + [Н] →Н2О + 2[ ],
where [ ] – free space on the surface of the catalyst; formation of methane (steps 4 – 7) is fast and
formation of water (steps 8–9) is slow.
Conclusion
A series of the Ni-Fe catalysts were prepared by the co-precipitation of the hydroxides. All
samples were reduced in the same conditions, and they were applied to the methane production
from CO2 and H2. Among the tested catalysts, Ni80Fe20 showed the best catalytic performance in
terms of conversion of CO2 and yield for CH4. It has been shown that the conversion of CO2 to
methane is significantly increased over the bimetallic nickel-iron catalysts compared to the pure
nickel catalyst. The experiments illustrate that the best catalysts have a Ni/Fe ratio above 4. TD
MS analysis of active and inactive samples’ surface showed that CO2 hydrogenation process over
Ni–Fe catalysts has the mechanism that does not involve oxygen-containing intermediates. Based
on results of catalytic performance and thermal desorption one can suggest that process of CO2
hydrogenation over Ni-Fe catalysts proceeds via direct hydrogenation of C atom (formed in CO2
dissociation) to CH4.
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ДОСЛІДЖЕННЯ ЧАСТИНОК НА ПОВЕРХНІ Ni-Fe
КАТАЛІЗАТОРІВ ГІДРОГЕНУВАННЯ СО2 МЕТОДОМ
ТД МС АНАЛІЗУ
Р. Мешкініфар, А. Дяченко, О. Бєда, О. Іщенко
Київський національний університет імені Тараса Шевченка
вул. Володимирська, 64, Київ, 01601, Україна
r.meshkinifar@gmail.com
Методом термопрограмованої десорбційної мас-спектрометрії (ТД МС) досліджено
стан поверхні Ni-Fe каталізаторів реакції гідрогенування СО2. На ТД спектрах
зареєстровано десорбцію частинок CO2 (m/z = 44), CO (m/z = 28) та H2O (m/z = 18) з
поверхні зразків, що проявили високу та низьку каталітичну активність у реакції
гідрогенування СО2. Проміжні сполуки CHO*, CH2O
* не спостерігалися на ТД профілях для
всіх досліджуваних зразків. На основі результатів каталітичної активності та термічної
десорбції зроблено припущення, що процес конверсії СО2 в метан на Ni-Fe каталізаторах
відбувається через пряме гідрогенування карбону без утворення проміжних кисневмісних
сполук.
110
ИССЛЕДОВАНИЕ ЧАСТИЦ НА ПОВЕРХНОСТИ Ni-Fe
КАТАЛИЗАТОРОВ ГИДРОГЕНИРОВАНИЯ СО2 МЕТОДОМ
ТД МС АНАЛИЗА
Р. Мешкинифар, А. Дяченко, А. Беда, Е. Ищенко
Киевский национальный университет имени Тараса Шевченко
ул. Владимирская, 64, Киев, 01601, Украина
r.meshkinifar@gmail.com
Методом термопрограмированной десорбционной масс-спектрометрии (ТД МС)
исследовано состояние поверхности Ni-Fe катализаторов реакции гидрогенирования СО2.
По ТД спектрах зарегистрировано десорбцию частичек CO2 (m/z = 44), CO (m/z = 28) та
H2O (m/z = 18) с поверхности образцов, которые показали высокую и низкую активность в
реакции гидрогенирования СО2. Образование промежуточных соединений CHO*, CH2O
*
не наблюдалось ни для одного из исследованных образцов. Из полученных результатов по
изучению каталитической активности и термической десорбции сделано предположение,
что процесс конверсии СО2 в метан на Ni-Fe катализаторах происходит путем прямого
гидрогенирования атомарного углерода без образования промежуточных
кислородсодержащих соединений.
|
| id | oai:ojs.pkp.sfu.ca:article-639 |
| institution | Surface |
| keywords_txt_mv | keywords |
| language | English |
| last_indexed | 2025-12-02T15:19:44Z |
| publishDate | 2017 |
| publisher | Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine |
| record_format | ojs |
| resource_txt_mv | surfacezbircomua/e2/396ffd65d76f09c07a4bf50634e50de2.pdf |
| spelling | oai:ojs.pkp.sfu.ca:article-6392018-12-01T11:32:03Z Surface species investigation of Ni-Fe catalysts of CO2 hydrogenation by TD MS analysis Исследование частиц на поверхности Ni-Fe катализаторов гидрогенирования СО2 методом ТД МС анализа Дослідження частинок на поверхні Ni-Fe каталізаторів гідрогенування СО2 методом ТД МС аналізу Meshkini Far, R. Dyachenko, A. Bieda, O. Ischenko, O. Ni-Fe catalysts CO2 hydrogenation catalytic activity TD-MS analysis The condition of Ni-Fe catalysts’ surface was investigated by the method of thermally programmed desorption with mass spectral analysis of desorbed particles (TD MS). TD spectra indicated the desorption of CO2 (m/z = 44), CO (m/z = 28) and H2O (m/z = 18) particles from the surface of samples with high and low catalytic activity in the reaction of CO2 hydrogenation. Intermediate compounds CHO*, CH2O* were not observed in the TD profiles for all investigated catalysts. On the basis of catalytic performance results and thermal desorption data it can be suggested that process of CO2 hydrogenation over Ni-Fe catalysts proceeds via direct hydrogenation of CO2 to CH4. Методом термопрограмированной десорбционной масс-спектрометрии (ТД МС) исследовано состояние поверхности Ni-Fe катализаторов реакции гидрогенирования СО2. По ТД спектрах зарегистрировано десорбцию частичек CO2 (m/z = 44), CO (m/z = 28) та H2O (m/z = 18) с поверхности образцов, которые показали высокую и низкую активность в реакции гидрогенирования  СО2. Образование промежуточных соединений CHO*, CH2O* не наблюдалось ни для одного из исследованных образцов. Из полученных результатов по изучению каталитической активности и термической десорбции сделано предположение, что процесс конверсии СО2 в метан на Ni-Fe катализаторах происходит путем прямого гидрогенирования атомарного углерода без образования промежуточных кислородсодержащих соединений. Методом термопрограмованої десорбційної мас-спектрометрії (ТД МС) досліджено стан поверхні Ni-Fe каталізаторів реакції гідрогенування СО2. На ТД спектрах зареєстровано десорбцію частинок CO2 (m/z = 44), CO (m/z = 28) та H2O (m/z = 18) з поверхні зразків, що проявили високу та низьку каталітичну активність у реакції гідрогенування СО2. Проміжні сполуки CHO*, CH2O* не спостерігалися на ТД профілях для всіх досліджуваних зразків. На основі результатів каталітичної активності та термічної десорбції зроблено припущення, що процес конверсії СО2 в метан на Ni-Fe каталізаторах відбувається через пряме гідрогенування карбону без утворення проміжних кисневмісних сполук. Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine 2017-10-08 Article Article application/pdf https://surfacezbir.com.ua/index.php/surface/article/view/639 10.15407/Surface.2017.09.104 Surface; No. 9(24) (2017): Surface; 104-110 Поверхность; № 9(24) (2017): Поверхность; 104-110 Поверхня; № 9(24) (2017): Поверхня; 104-110 3154-8091 3154-8083 10.15407/Surface.2017.09 en https://surfacezbir.com.ua/index.php/surface/article/view/639/639 Авторське право (c) 2017 R. Meshkini Far, A. Dyachenko, O. Bieda, O. Ischenko |
| spellingShingle | Meshkini Far, R. Dyachenko, A. Bieda, O. Ischenko, O. Дослідження частинок на поверхні Ni-Fe каталізаторів гідрогенування СО2 методом ТД МС аналізу |
| title | Дослідження частинок на поверхні Ni-Fe каталізаторів гідрогенування СО2 методом ТД МС аналізу |
| title_alt | Surface species investigation of Ni-Fe catalysts of CO2 hydrogenation by TD MS analysis Исследование частиц на поверхности Ni-Fe катализаторов гидрогенирования СО2 методом ТД МС анализа |
| title_full | Дослідження частинок на поверхні Ni-Fe каталізаторів гідрогенування СО2 методом ТД МС аналізу |
| title_fullStr | Дослідження частинок на поверхні Ni-Fe каталізаторів гідрогенування СО2 методом ТД МС аналізу |
| title_full_unstemmed | Дослідження частинок на поверхні Ni-Fe каталізаторів гідрогенування СО2 методом ТД МС аналізу |
| title_short | Дослідження частинок на поверхні Ni-Fe каталізаторів гідрогенування СО2 методом ТД МС аналізу |
| title_sort | дослідження частинок на поверхні ni-fe каталізаторів гідрогенування со2 методом тд мс аналізу |
| topic_facet | Ni-Fe catalysts CO2 hydrogenation catalytic activity TD-MS analysis |
| url | https://surfacezbir.com.ua/index.php/surface/article/view/639 |
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