An active and stable Ni/Al2O3 nanosheet catalyst for dry reforming of CH4

Article abstract of DOI:10.1039/c5ra11461f

A highly active and stable nano structured Ni/Al₂O₃ catalyst was developed by a simple two-step hydrothermal method. The obtained Ni/Al₂O₃ catalyst exhibited leaf-like nanosheets with ～5 nm thickness, and realized CH₄ conversion as high as 91.3% at 1073 K with excellent stability in the dry reforming of methane.

Full text of DOI:10.1039/c5ra11461f

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An active and stable Ni/Al O nanosheet catalyst for dry
2
3
reforming of CH4
Lin Zhang and Yi Zhang *
Received 00th January 20xx,
Accepted 00th January 20xx
DOI: 10.1039/x0xx00000x
www.rsc.org/
7
A highly active and stable nano structured Ni/Al
developed by a simple two-step hydrothermal method. The supported catalyst, prepared by modification of silica surface,
obtained Ni/Al catalyst exhibited leaf-like nanosheet with ~5 realized excellent stability during dry reforming reaction, because
nm thickness, and realized CH
2 3
O catalyst was Meanwhile, as our previously reported, the highly dispersed Ni
2
O
3
4
conversion as high as 91.3% at its smaller and stable Ni particles successfully prevented carbon
1
073K with excellent stability in dry reforming of methane.
deposition. However, the activity of these catalysts was always
damaged by coverage of Ni active sits or lower reducibility of
supported nickel.
As the demand for alternative energy resources increases
owing to depletion of crude oil supplies, methane has received
much attention because reserves of methane are larger than that of
On the other hand, the hydrothermal method has been
referred to as a versatile, low cost and environmentally friendly
method for the preparation of catalytic materials with different size
and morphology. Particles produced by hydrothermal synthesis are
1
, 2
crude oil.
Due to both energy and environmental reasons, the
reforming of methane with carbon dioxide to produce synthesis
3
-5
25
gas, CO and H , has received significant attention in recent years.
2
high purity, uniform dispersion and good crystal form. However,
these advantages always form abundant solid solution of active
phase and support, leading to extremely strong interaction
between the active metal and support, resulting in lower activity of
obtained catalysts due to the poor reducibility of supported metals.
Herein, a two-step hydrothermal process was developed to
synthesize the unique leaf-like nanostructured Ni/Al O (signed as
Considerable research efforts have been focused on the
development of active and thermodynamically stable catalysts for
the CO reforming of CH . It has been proved that supported noble
2
4
metal catalysts have promising catalytic performances and low
6
–12
sensitivities to carbon deposition.
However, concerning the
limited resources, numerous researches focused on non-noble
metal catalysts. Series of research papers have reported that
supported group VIII metals are good catalysts for dry reforming of
2
3
Ni/Al O (T)) catalyst with high activity and stability in dry reforming
2
3
of methane. It is believed that the Ni(OH) nanoparticles, prepared
2
1
3-19
methane.
A large number of publications indicate that
by first-step hydrothermal process, would be partially dissolved to
adjust the environment of the second hydrothermal synthesis,
contributing to forming unique morphology of obtained Ni/Al O
supported nickel catalysts exhibited high catalytic activity in dry
reforming of methane. The greatest problem of nickel-based
catalysts is the deactivation due to carbon deposition and Ni
particle sintering.
2
3
catalyst. On the other hand, the residual Ni(OH)2 nanoparticles
would provide the precursors of NiO with better reducibility, which
would be anchored by solid solution of dissolved Ni(OH)2
nanoparticles and formed Al O , contributing to excellent thermal
It was well reported that smaller Ni particles had a better
2
0-23
ability to prevent coke formation.
However, for supported
2
3
catalysts, the metal particles tend to aggregate during the reaction
process, which leads to lower catalytic activity and coke
stability of obtained catalyst. The products were collected and
purified by repeated centrifugation and then dried at 393 K for 2 h.
Calcination step was carried out by slowly increasing temperature
from room temperature to 773 K (2 K/min) and keeping at 773 K for
2
4
formation. Lee et al. developed highly coke-resistant Ni catalysts
2
by coating the Ni/nano-sphere SiO catalyst with silica overlayers.
2
The silica overlayer prevents the small Ni nanoparticles from
sintering, and successfully suppresses the coke formation.
3
h. For characterization of reduced catalysts, the calcined catalysts
were reduced by pure hydrogen at 1073 K for 2 h and then
passivated by 1% O in N to form a metal oxide layer on the surface
2
2
of metal particle in order to preventing oxidation of nickel metal
when the catalysts were exposed to air. For comparison, another
two Ni/Al O catalysts were prepared by one-step hydrothermal
2
3
(
(
signed as Ni/Al O (O)) and conventional impregnation method
2 3
signed as Ni/Al O (I)).
2
3
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The morphology of the fresh catalysts was determined by Microscopy (AFM) image and analysis proved the thickness of
Scanning Electron Microscopy (SEM). As shown in Fig. 1a, the obtained Ni/Al (T) catalyst was in range of 4.5-5.0 nm (Figure 1e).
Ni/Al (T) exhibited significant different morphology to other However, large bulk was observed in SEM images of Ni/Al (O)
(T) catalyst, as shown in Fig 1 b and c. Furthermore,
2
O
3
2
O
3
2 3
O
catalysts as leafy-like nanosheets (~700 nm in length, ~150 nm in and Ni/Al
2 3
O
width and ~5 nm in thickness). Meanwhile, the Atomic Force
2 3 2 3 2 3 2 3
Fig.1 SEM images of the various catalysts: (a) Ni/Al O (T), (b) Ni/Al O (O) and (c) Ni/Al O (I); (d) Pore distribution of obtained catalysts; (e) AFM image and analysis of Ni/Al O (T)
catalyst
the results of N
in Table S1†. As compared in Table S1†, the BET surface area and of Ni(OH)
pore volume of Ni/Al2O3 (T) catalyst was much higher than that of during calcination step. However, as shown in Fig. 2c, after
other two catalysts. The pore size distribution of Ni/Al (T) was reduction step, the homogeneous nickel metal clusters were
mainly concentrated at 2.4 nm (Fig 1d and Table S1†), which was formed with a diameter of 10 nm, which consisted of several Ni
smaller than that of Ni/Al (O) and Ni/Al (I) and contributed to particles with 2 nm diameter. The nickel clusters of Ni/Al (T)
the larger specific surface area. It is considered that the leaf-like catalyst were confined in specific area and effectively separated
nanosheet structure and large pore volume would provide large from each other, which were quite different to that of Ni/Al (O)
channel to improve the diffusion of reactants and products, and Ni/Al (I) catalysts. It is believed that the well confined and
improving the activity of the Ni/Al (T) catalyst. Meanwhile, the separated Ni clusters would prevent sintering of Ni active phase
large surface area would promote the dispersion of supported during dry reforming of methane, contributing to excellent stability
nickel, leading to high activity and stability. The morphology of of this catalyst. The morphology of metallic Ni particles of Ni/Al
2
adsorption-desorption analysis were summarized Ni(OH)
2
nanoparticles were partially dissolved and the residual part
2
nanoparticles formed the extremely small NiO particles
2
O
3
2
O
3
2
O
3
2 3
O
2 3
O
2
O
3
2
O
3
2
O
3
calcined and reduced catalysts was also detected by Transmission (T) catalyst was also determined by HRTEM. The nanoparticle
electron microscopy (TEM) and High-resolution transmission consisted of two different crystalline, where the lattice fringes of
electron microscopy (HRTEM), and the images were illustrated in the core crystalline was 0.203 nm, assigned to the (111) plane of
Fig. 2. For the Ni/Al
and passivated catalyst (Fig 2 c) exhibited leaf like nanosheet 0.24 nm, assigned to the (311) plane of NiAl
structure, which is quite different to Ni/Al (O) and Ni/Al (I) considered that the dissolved Ni(OH) particles formed the NiAl
catalysts. As shown in Fig 2 a (insert), clear lattice fringes with a d- to anchor the Ni metal particle formed from residual Ni(OH)
spacing of 0.197 nm indexed to the [400] plane of γ-Al particles. Meanwhile, the dissolved part of Ni(OH)
leaves are along [400] around environment of Ni(OH) particles in second hydrothermal
system leading to synthesis of leaf-like nanosheets of Al
The morphology of passivated Ni/Al (T) catalyst was also
T) catalyst were extremely small with less than 1 nm diameter. As detected by Scanning Transmission Electron Microscopy (STEM). As
the precursors of NiO for Ni/Al (T) catalyst were Ni(OH) shown in Fig. 3a, the STEM image of the catalyst exhibited similar
2
O
3
(T) catalyst, both of calcined (Fig 2a and 2b) the metallic Ni, and the lattice fringes around the metallic Ni was
2
O
4
(Fig. 2d). It is
2
O
3
2
O
3
2
2
O
4
2
2
O
3
,
2
modified the
indicating that the growths of the Al
directions.
2
O
3
2
2
3
O .
As can be seen in Fig. 2b, the NiO particles of calcined Ni/Al
2
O
3
2 3
O
(
2
O
3
2
nanoparticles formed by the first hydrothermal process, it is images to Fig 2c, as leaf-like nanosheets contained the separated Ni
considered that during the second hydrothermal process the added clusters. The chemical composition of this catalyst was determined
2
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by the energy-dispersive spectroscopy (EDS) elemental mapping several nickel particles (bright green colour) and surrounded by
analysis. As shown in Fig. 3b-d, Ni, O and Al mapping images clearly solid solution of Ni and Al
reveal chemical composition and distribution. Ni clusters consist of
2 3
O (light green colour).
2 3 2 3 2 3 2 3
Fig.2 TEM images of various catalysts. (a and b):fresh Ni/Al O (T), (c and d): passivated Ni/Al O (T), (e): passivated Ni/Al O (O), (f): passivated Ni/Al O (I).
2
6
2
NiAl O
4
.
From Fig. S2b†, the metallic Ni peaks appeared in all
or NiO have been
passivated catalysts. This suggests that the AlNiO
4
reduced by hydrogen to form metallic Ni particles. No obvious
difference was observed among three kinds of catalysts from
patterns of fresh and passivated catalysts. Therefore, the
reducibility of the catalysts is necessary to obtain information about
the metal-support interaction.
H
2
-Temperature Programmed Reduction (H
various calcined catalysts were shown in Fig. S3†. Besides a very
small peak at 623K, the Ni/Al (I) exhibited two main reduction
peaks at 788K and 1053K of. For Ni/Al (O), there was a big H
consumption peak at 1053K with two shoulders at 733K and 900K
respectively. However, for Ni/Al (T), there are a broad peak
located at 643K and two strong reduction peaks located at 923K
2
-TPR) profiles of
2 3
O
2
O
3
2
2
O
3
2
7-28
and 1140K. According to previous literatures,
the peaks
centered at different temperature can be related to different NiO
species, namely free NiO phase located at low reduction
Fig.3 STEM/EDS micrographs displaying the morphologies of Ni incorporated onto the
surface of Al after passivation. STEM image of Ni/Al2O3 (T) (a); Elemental mapping
temperature, fixed NiO phase and NiAl
2
O
4
phase located at high
(T)
2 3
O
reduction temperature. Therefore, it is believed that Ni/Al
2 3
O
analysis: Ni (b); O (c); Al (d).
catalyst contained the most of free NiO species and the strongest
metal–support interaction in this study, due to its special
From the observed morphologies of the samples at different
stages of the second hydrothermal process (Fig S1†, detailed
2 3
preparation method and leaf-like nanosheet structure. For Ni/Al O
(
O), the one-step hydrothermal process resulted in the worst
discussion), it is believed that the Ni(OH)
partially dissolved into the solution of second hydrothermal
reaction, leading to modifying the crystallization of Al . The
Ni(OH) particles underwent a part-dissolution process in the
second hydrothermal reaction and leaf-like nanosheet structure of
Ni/Al (T) catalyst was formed via oriented attachment growth of
crystals.
2
particles (5nm) would
2
9-32
reducibility in this study. As reported by references,
the free
NiO species can form more active sites after reduction, stronger
metal–support interaction is advantageous to better coke-
resistance of the catalyst, and those would contribute to high
2
O
3
2
activity and excellent stability of Ni/Al
methane.
2 3
O (T) during dry reforming of
2 3
O
The obtained catalysts were tested in dry reforming of methane.
The dry reforming of methane was carried out at 973 K under
X-ray Diffraction (XRD) patterns of the fresh and passivated
catalysts are shown in Fig. S2†. For various calcined catalysts, no
diffraction peaks of NiO were observed in the XRD patterns, due to
high dispersion of NiO or transformation of most NiO phase to
4 2
atmospheric pressure (Ar/CH /CO =4/48/48, where Ar is inner
3
−1 −1
2 3 4
reference, GHSV= 21000cm ·g ·h ). Ni/Al O (T) realized 76% CH
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conversion (Fig 4a), which was much higher than that of Ni/Al
and very close to equilibrium conversion at 973K. The Ni/Al
exhibited 70% CH
the other hand, both Ni/Al
2
O
3
(O) resistance of carbon deposition during the dry reforming of
2 3
O (I) methane. It is believed that the novel leaf-like nanosheet structure
4
conversion followed by quick deactivation. On of the Ni/Al
2 3
O (T) catalyst resulted in stable nickel particle and
2
O
3
(T) and Ni/Al (O) showed excellent more active sites, contributing to remarkable reaction performance.
2 3
O
stability during 10 hrs reaction. It is considered that more nickel and On the other hand, the leaf-like structure could accommodate the
alumina solid solution was formed on these two catalysts due to the gaseous reactants with more exposed Ni active sites than
hydrothermal preparation method, which contributed to improving conventional supported catalysts, further contributing to the
the stability of obtained catalyst. Meanwhile, because Ni/Al
contained more free NiO species, as proved by H -TPR, more active
sits would be formed after reduction step, contributing to high CH
conversion. The conversion of CO is similar to CH conversion for Ni/Al
three catalysts. In all cases, CH conversions were lower than the small nickel particles, dispersed on the leafy-like nanosheet
corresponding CO conversion, due to the reverse water-gas shift substrate, and the deposited carbon was not found on this catalyst.
2 3
O (T) catalytic activity and stability.
2
The spent catalysts after 10 h reaction were characterized by
several characterizations. As shown in Fig.5a, the TEM images of
4
2
4
2 3
O (T) showed that the nickel clusters consisted of several
4
2
3
3
(
RWGS) reaction during CH /CO reforming reaction.
Therefore, comparing to TEM images of the passivated catalyst (Fig.
c), it is indicated that the Ni nanoparticles firmly immobilized in
the Al O support, effectively inhibiting the aggregation,
4
2
2
2
3
contributing to the best stability in this study. In comparison, nickel
particles on Ni/Al O (O) and Ni/Al O (I) obviously aggregated to
2
3
2
3
large particles and deposited carbon species appeared in the TEM
images (Fig. 5b and c). The XRD patterns of various used catalysts
are illustrated in Fig. S6†. Compared with the XRD patterns of
Ni/Al O (T) and Ni/Al O (O), the Ni/Al O (I) exhibits larger metallic
2
3
2
3
2 3
Ni peaks and strong diffraction peaks attributed to deposited
carbon species, indicating the extremely sintering of nickel particles
and more carbon deposition.
The amounts of carbon deposition of three catalysts were
investigated by TG/DTA, as shown in Fig. S7†. The carbon
deposition could occur on Ni-based catalysts in various forms, such
as atomic carbon, amorphous carbon and graphitic carbon, which
3
4,
can be gasified to CO in O atmosphere at different temperature.
2
2
3
5
From TG-DTA profiles (Fig. S7†), two types of carbon deposits are
identified on Ni/Al O catalyst, which correspond to the much
2
3
reactive amorphous carbon at low temperature and the less
3
4, 35
reactive graphitic carbon at high temperature.
From DTA
curves (Fig S7a†), for the Ni/Al O (I) catalyst, beside one weak
2
3
exothermic peak at 608K, there was a strong peak at 903K, which
indicated that numerous graphitic carbon and little amorphous
carbon deposited on the Ni/Al O (I) during activity testing. For
2
3
Ni/Al O (O), two exothermic peaks appeared at 613K and 923K
2
3
were significantly weaker than those of Ni/Al O (I), indicating that
2
3
less coke deposited on Ni/Al O (O). Furthermore, the exothermic
2
3
peak of lower temperature was stronger than that of higher
temperature, indicating that the active deposited carbon was more
than less reactive graphic carbon, contributing to the stability of
Fig.4 Reaction performance of various catalysts at 973K (a) and catalytic testing of
Ni/Al (T) at 1073K (b). Reaction conditions: Ar/CH /CO =4/48/48, Catalyst: 0.1g,
GHSV=21000cm ·g ·h
O
2 3
4
2
3
−1 −1
Ni/Al
83K and 823K of Ni/Al
was deposited on the surface of the Ni/Al
2
O
3
(O) catalyst. The two extremely weak exothermic peaks at
(T) indicated that the much less carbon
(T), promoting the
5
2 3
O
To further investigate the stability of the Ni/Al
/CO reforming at 1073K was carried out for 50 h. As shown in
Fig.4b, the ratio of H /CO was about 0.92 and the conversion of CH
reached 91.3%, which is close to the thermodynamic equilibrium
conversion at 1073K (presented in Fig.4a). No decline of CH
2 3
O (T), the
2 3
O
CH
4
2
best stability of this catalyst in this study. Generally, samples
absorbed gas from the air, resulting in the weight loss before 373K.
As the TG curves illustrated in Fig. S7b†, the weight loss of carbon
2
4
4
2 3
deposition for used Ni/Al O (T) was only 6.26%, which is much
conversion was observed during the whole reaction, indicating the
excellent stability. The spent catalysts after 50 h reaction were
characterized by TEM and TG/DTA. As shown in Fig. S4†, the TEM
lower than that of other two catalysts (11.48% and 21.16%
respectively). It is considered that the reconstitution of the firstly
2
synthesized Ni(OH) nanoparticles contributes to formation of
image of used Ni/Al
on this catalyst. Meanwhile, the TG/DTA profiles (Fig. S5†) show
that the weight loss of Ni/Al (T) is only 5%, implying its excellent
2 3
O (T), no obvious deposited carbon was found
highly dispersed Ni metal particles via forming solid solution around
the nickel particles, which suppresses the sintering of Ni particles
and leads to less carbon deposition during dry reforming of
2 3
O
4
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2 3 2 3 2 3
Fig.5 TEM images of used catalysts: (a) Ni/Al O (T), (b) Ni/Al O (O), (c) Ni/Al O (I)
methane. Meanwhile, during the secondary hydrothermal process,
the partial dissolution and re-crystallization of Ni(OH) successfully
adjusts the interaction between the supported Ni and alumina
support, as proved by H -TPR, which might generate different
interface of supported Ni and alumina support, contributing to
resistance of carbon deposition. Therefore, the Ni/Al (T) catalyst
3
4
5
6
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RSC Advances
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DOI: 10.1039/C5RA11461F
An active and stable Ni/Al O nanosheet catalyst for dry reforming of
2
3
methane
Lin Zhang and Yi Zhang *
A highly active and stable leaf-like nanosheet Ni/Al O catalyst was developed by a simple
2
3
two-step hydrothermal method.