Dual-Function Cobalt–Nickel Nanoparticles Tailored for High-Temperature Induction-Heated Steam Methane Reforming

Article abstract of DOI:10.1002/anie.201804832

The tailored chemical synthesis of binary and ternary alloy nanoparticles with a uniform elemental composition is presented. Their dual use as magnetic susceptors for induction heating and catalytic agent for steam reforming of methane to produce hydrogen at temperatures near and above 800 °C is demonstrated. The heating and catalytic performance of two chemically synthesized samples of CoNi and Cu?CoNi are compared and held against a traditional Ni-based reforming catalyst. The structural, magnetic, and catalytic properties of the samples were characterized by X-ray diffraction, elemental analysis, magnetometry, and reactivity measurements. For induction-heated catalysts, the conversion rate of methane is limited by chemical reactivity, as opposed to the case of traditional externally heated reformers where heat transport limitations are the limiting factor. Catalyst production by the synthetic route allows controlled doping with miniscule concentrations of auxiliary metals.

Full text of DOI:10.1002/anie.201804832

A Journal of the Gesellschaft Deutscher Chemiker
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Accepted Article
Title: Dual Function Cobalt-Nickel Nanoparticles Tailored for High-
Temperature Induction-Heated Steam Methane Reforming
Authors: Morten Gotthold Vinum, Mads Radmer Almind, Jakob S.
Engbæk, Søren B. Vendelbo, Mikkel Fougt Hansen, Cathrine
Frandsen, Jesper Bendix, and Peter Mølgaard Mortensen
This manuscript has been accepted after peer review and appears as an
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of the final Version of Record (VoR). This work is currently citable by
using the Digital Object Identifier (DOI) given below. The VoR will be
published online in Early View as soon as possible and may be different
to this Accepted Article as a result of editing. Readers should obtain
the VoR from the journal website shown below when it is published
to ensure accuracy of information. The authors are responsible for the
content of this Accepted Article.
To be cited as: Angew. Chem. Int. Ed. 10.1002/anie.201804832
Angew. Chem. 10.1002/ange.201804832
Link to VoR: http://dx.doi.org/10.1002/anie.201804832
http://dx.doi.org/10.1002/ange.201804832

10.1002/anie.201804832
Angewandte Chemie International Edition
COMMUNICATION
Dual Function Cobalt-Nickel Nanoparticles Tailored for High-
Temperature Induction-Heated Steam Methane Reforming**
Morten G. Vinum,* Mads R. Almind, Jakob S. Engbæk, Søren B. Vendelbo, Mikkel F. Hansen, Cathrine
Frandsen, Jesper Bendix,* and Peter M. Mortensen*
Abstract: We present the tailored chemical synthesis of binary and ternary
alloy nanoparticles with a uniform elemental composition and demonstrate
their dual use as magnetic susceptors for induction heating and catalytic
agent for steam reforming of methane to produce hydrogen at temperatures
near and above 800C. The heating and catalytic performance of two
chemically synthesized samples of CoNi and Cu⊂CoNi, are compared
and held against a traditional Ni-based reforming catalyst. The structural,
magnetic and catalytic properties of the samples were characterized by X-
ray diffraction, elemental analysis, magnetometry and reactivity
measurements. Notably, for induction-heated catalysts, the conversion rate
of methane is shown to be limited by chemical reactivity, as opposed to the
case of traditional externally heated reformers where heat transport
limitations are the limiting factor. Catalyst production via the synthetic
route allows for controlled doping with miniscule concentrations of
auxiliary metals, which facilitates activity-modification by chemical tuning
to synchronize the catalyst material to heating input.
and nuclear energy. The most affordable and efficient way to generate
hydrogen is still various forms of steam reforming of hydrocarbons
from fossil fuels.[9] The SMR takes place according to
CH4 + H2O ⇌ 3H2 + CO (∆퐻° = 206.15 kJ mol-1)
CO + H2O ⇌ H2 + CO2 (∆퐻° = −41.16 kJ mol-1)
(1)
(2)
This overall endothermic reaction presents a challenge as it is only
thermodynamically favored at temperatures approaching 700C at
ambient conditions, and even higher temperatures of 950C are needed
in industry due to the high pressures of operation.[10]
A typical SMR plant for production of hydrogen generally
consists of a pre-reformer followed by a tubular reformer, a shift
converter, and final product purification (typically done by pressure
swing adsorption (PSA)) in combination with expensive heat-exchange
coils to minimize heat loss.[11] A long-standing challenge in hydrogen
production has been the excessive heating needed in the reforming
section of the current design, which, due to costly waste-heat sections,
favors large-scale plants to achieve a feasible reforming economy.
Usually, energy delivered to the reactor bed from the fired section is
only around 50%, the rest is recovered in the flue gas.[10,12] This
however dictates, that a significant amount of energy is spent outside
of the actual reaction chamber. Additionally, the start-up time of such
plants is often on the order of a few days to ensure controlled heating
of the large tubes with minimum risk of tube rupture. In stark contrast,
induction heating provides rapid and efficient heating of ferromagnetic
materials, and potentially the heat can be delivered directly in the
catalyst, if such a “magnetic” catalyst can be realized. This requires
special radiofrequency transparent reactors to avoid shielding effects
between the catalyst and the induction coil. In a future hydrogen
economy, we therefore envision induction-heated reforming as a small-
scale hydrogen production technology with a fast start-up for ad hoc
on-site supply of hydrogen.
Direct heating of magnetic nanoparticles (NPs) by magnetic
induction, including using magnetic hysteresis heating, holds many
potential advantages over conventional heating as it allows for a vast
number of new approaches to otherwise difficult tasks. The most
prominent of these are drug release,[1,2] control of single-cell
functions,[3] and disease treatment by hyperthermia.[4,5] While a
collective feature of all these applications is the aim towards medical
use, only few examples exist of industrial applications of magnetically
heated NPs.[6] Herein, we present the preparation and implementation
of a novel nanostructured material for hydrogen production via
endothermic steam reforming of methane (SMR) using solely induction
heating as energy source.[7]
Hydrogen is by far the most produced chemical worldwide on a
molar basis.[8] To accommodate an ever-growing demand, efforts have
been made to generate hydrogen from biofuels, electrolysis, wind, solar,
Previously, induction heating of ferromagnetic Fe-based NPs
was utilized in a liquid phase organic synthesis flow reactor in a series
of pioneering studies,[13–15] albeit the NPs were only used for heating
and did not supply a catalytic function. Others have later made research
into magnetic zeolites and related systems, where NiFe-based particles
may also play a catalytic role.[16,17] More recently, others reported iron-
based core-shell NPs doped with precious metals as candidates for
induction heated heterogeneous catalysis.[18,19] However, in case of
SMR with reaction temperatures around 800 °C, iron with a Curie
temperature, TC, of 770 °C is not suitable as magnetic susceptor. The
only element with a higher TC than iron is cobalt (TC 1115 °C)[20] and
hence for induction heated SMR, the magnetic susceptor must be based
on Co and alloys thereof.
[*]
M. G. Vinum, Dr. P. M. Mortensen
Haldor Topsøe A/S
Nymøllevej 55, 2800 Kgs. Lyngby (Denmark)
E-mail:
morten.vinum@chem.ku.dk
pmor@topsoe.com
M. G. Vinum, Prof. Dr. J. Bendix
Department of Chemistry, University of Copenhagen
2100 Copenhagen (Denmark)
E-mail:
bendix@kiku.dk
M. R. Almind, Prof. Dr. C. Frandsen
DTU Physics, Technical University of Denmark
2800 Kgs. Lyngby (Denmark)
Dr. J. S. Engbæk, Dr. S. B. Vendelbo
Danish Technological Institute
2630 Taastrup (Denmark)
Dr. M. F. Hansen
DTU Nanotech, Technical University of Denmark
2800 Kgs. Lyngby (Denmark)
Oxidation of Co readily takes place at the high temperatures and
partial pressures of water relevant to the SMR process, and a
significant challenge is to avoid oxidation of Co as this leads to the
formation of antiferro- and paramagnetic phases.[21,22] Alloying with Ni
provides a dual solution to this as Ni is an excellent catalyst for
endothermic SMR, and Ni stabilizes the Co phase against oxidation
while maintaining activities similar to that of pure Ni.[21] Recently, we
had some success with this idea in a proof-of-concept paper, showing
[**]
This work was partly funded by The University of Copenhagen,
Haldor Topsøe A/S, the CoNeXT project and Innovation Fund
Denmark (IFD) under File No. 5160-00004B. A PCT patent has
been approved based on the results obtained.
Supporting information for this article is given via a link at the end of
the document.
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10.1002/anie.201804832
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that it was indeed possible to heat such alloyed NPs to temperatures
approaching the desired range, and to produce hydrogen at these
elevated temperatures. However, due to the serendipity of sequential
impregnation used in the previous study, control over the microscopic
metal distribution had to be renounced, evidenced by the large
differences found in alloy compositions in that study, leaving only a
small fraction with high TC and a very small hysteresis opening (vide
infra) accessible for the purpose of heating.[23–25]
Herein, to take control at the molecular level, we conceptually
changed the approach to catalyst manufacture, by preparing both active
NPs and inert carrier via a chemical synthesis route, with the aim of
producing more stable and uniform NPs, accessible in the desired
temperature regime. Forming the catalyst precursor in solution and
then precipitating it by addition of base, guaranteed the homogeneity of
the material. Subsequently, the material was reduced, hereby directly
producing catalytic nanoparticles within a porous non-active carrier
material. To benchmark the activity of the formed catalyst, we also
synthesized a traditional Ni catalyst on MgAl2O4 support via the same
route with a loading of 15 wt.% Ni (1) as a reference, to mimic
commercially available reforming catalyst,[10] denoted Ni-ref (Table S1,
Fig. S1).
The synthetic procedure (see SI and Fig. S2) uniformly gave a
homogeneous compound, which could be tuned to accommodate a vast
range of metals at different ratios. The initial precipitate was shown by
XRD to consist of a spinel-type phase of MyCo(1-x-½y)Ni(x-½y)Al2O4
(where M = Cr, Mn, Fe, Cu as shown in Table S1, Fig. S3). Here, we
chose to focus on just two chemically synthesized samples, one un-
doped sample with x = 0.5 (2a) hereafter CoNi, and a Cu-doped sample
Figure 2. Weight percentage of Co throughout individual NPs in CoNi. The
bottom graph represents the sample studied in a 300 h induction heated steam
reforming experiment, seen in Fig. 6. The dashed line at 50wt% represents the
nominal composition
addressed per sample) with an average Co content of each NP of 52.9
wt.% (5.8 wt.%) in sample CoNi (Fig. 2) and 52.9 wt.% (3.0 wt.%)
in sample Cu⊂CoNi (Fig. S7-S9), close to the stoichiometric ratio
defined by the synthetic route.
Measurements using
a traditional externally heated setup
dedicated for steam reforming activity measurements revealed a steam
reforming activity for CoNi of 40% of that for Ni-ref. Chemically
tuning the activity with miniscule dopings of Cu (Cu ⊂ CoNi)
increased the performance significantly to reach 55%. In terms of turn
over frequency (TOF) per exposed metal site (taking the size and metal
distribution into account), the TOF’s of CoNi and Cu⊂CoNi were
found to 75% and 91% of that of Ni-ref, respectively (Table 1). The
observation that miniscule doping with Cu promotes activity of Ni
catalysts in SMR concurs with literature[26] and additional results
Figure 1. Left: STEM-HAADF image of a freshly prepared sample of CoNi.
Right: Elemental mapping of Al (purple), O (teal), Co (red), and Ni (green) using EDS
analysis of the same sample. Co wt.% determined by EDS analysis for CoNi is
presented in Fig. 2.
Table 1. Selected properties of samples 1, 2a and 2b.
with x = 0.5 and y = 0.01 (2b) hereafter Cu ⊂ CoNi (Table 1).
Following reduction of both samples in hydrogen, peaks originating
from fcc-Co/Ni (Figs. S4 and S5) were identifiable in the XRD patterns
of both CoNi and Cu⊂CoNi indicating the formation of metallic NPs,
as well as -Al2O3 (both cubic and tetragonal phases) by the
degradation of the original spinel structure. No evidence of non-
reduced starting material was found in the final samples.
120 kV scanning transmission electron microscopy (STEM)
high-angle annular dark field (HAADF) images were used in
combination with electron dispersive X-ray spectroscopy (EDS) to map
and evaluate the nature and composition of the NPs of CoNi and Cu⊂
CoNi formed on the surface of the alumina support by the reduction
process. From this, an average length/width of ~44/~36 nm and
~54/~43 nm, were evaluated for CoNi and Cu⊂CoNi, respectively
(Fig. S6). These results are consistent with the crystallite sizes of 20-30
nm estimated from XRD analysis using the Scherrer equation,
considering the uncertainties associated with this (Table S1, see SI for
further comments).
Sample
(Name)
Composition
Activity[a]
TC
Ni–TOF[a]
[mol g-1 h-1]
[s-1]
15.0wt%Ni⊂MgAl2O4
Co0.5Ni0.5⊂Al2O3
0.36wt%Cu⊂2a
355C[b]
892C[b]
875C[b]
1
0.440
0.184
0.244
0.584
0.435
0.535
(Ni-ref)
2a
(CoNi)
2b
(Cu⊂CoNi)
[a]
[b]
Measured at 450C.
Estimated via the two-tangent method applied to the
magnetic moment vs. temperature plots (see SI and Fig. S10).
obtained by traditional activity measurements (Table S1). Any possible
support related effects on the activity was not studied here.
The magnetic moment of CoNi and Cu⊂CoNi was measured
versus temperature in a small applied magnetic field of 10 mT to
determine the effective Curie temperature of the samples as well as to
check for the presence of multiple magnetic phases (Fig. 3). At
temperatures below 800C, the nanomaterial acted as a ferromagnet
The EDS analysis revealed an even distribution of Ni and Co
throughout the nanoparticles (more than 40 NPs were individually
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–Bmax and back (Fig 4). From the measurements conducted on CoNi, it
is clear that WH is still appreciably different from zero at temperatures
above 800C at moderate values of Bmax. This suggests the possibility
of using magnetic hysteresis heating at and above this temperature.
Identical measurements on Cu⊂CoNi reveal a similar hysteretic
behavior which is not surprising given the similar magnetization curves
(Figs. S15-S16). A reactor setup dedicated for induction-heated SMR
was designed and used for the testing of these catalysts under operating
conditions (see SI). A reactor made of quartz was implemented to
avoid any magnetic shielding effects. Based on the composition of the
outlet gas, the SMR equilibrium temperature, energy transfer, and
conversion of feed was calculated. For both CoNi and Cu⊂CoNi, the
calculated energy transfer to the process gas was around 3-20 W·g-1,
(averaged over a sample mass of 10 g) as estimated from the change in
enthalpy, depending on the flow-rate of reactants however, the actual
transfer to the reactor may be higher due to heat losses associated with
the reactor insulation. In all measurements, a frequency of 69kHz and
field amplitudes of up to 42 mT was used. For simplicity, only flow
rates of 51 and 152 Nl·h-1 are shown in Fig. 5. For a full view see Figs.
S17 and S18.
Figure 3. Magnetic moment versus temperature of CoNi and Cu⊂CoNi. The
sample was measured in an applied magnetic field of Bapp = 10 mT at temperatures
decreasing from 950°C to 200°C at 5°C min-1. Apparent solid lines are actual data
points
with a slow decrease of the magnetic moment upon heating. Above this
temperature, the moment decreased more rapidly and reached a value
close to zero at the maximum measurement temperature of 950C.
Effective Curie temperatures for CoNi and Cu ⊂ CoNi were
Traditionally, the limiting factor on the reaction rate in industrial
type externally heated reformer tubes is not the catalyst activity but the
heat transfer to the catalyst.[21,27] This means that effectively only 10%,
determined to TC = 892C and 875C, respectively (see SI). The single
rapid decrease in moment, around 850 C or 825 C indicates a
homogenous material with a narrow alloy composition in both samples
in agreement with EDS results. The smaller TC for Cu⊂CoNi relative
to CoNi despite similar composition in EDS may be due to the small
content of nonmagnetic Cu which was not evaluated by EDS.
Moreover, hysteresis measurements of CoNi and Cu⊂CoNi in
maximum applied magnetic fields Bmax ranging from 5 mT to 55 mT
were conducted isothermally between temperatures of 200C and
950C in increments of 50C (Figs. S11-S14). The area of the
hysteresis loop defined as
Figure 5. Influence of methane-flow on the conversion of CH4 in the steam reforming
reaction for a gas mixture treated over CoNi (diamonds) and Cu⊂CoNi (triangles) as
a function of applied magnetic field. Inset: steam reforming equilibrium temperature
as function of methane conversion at the experimental conditions. Inlet temperature ≈
200C, S/C ≈ 2, P ≈ 0 bar gauge. Gas composition as explained in the text and SI
or less, of the catalyst activity is utilized, the rest being “lost” due to
transport restrictions of the heat flux in the reactor bed.[27]
Interestingly, the data for CoNi and Cu⊂CoNi showed the CH4
conversion increasing with magnetic field, until a certain point where
the increase in field is accompanied only by a small increase in H2. For
certain gas flows, this maximum is reached at full conversion
(equilibrium). The curvature observed on approaching equilibrium is
caused by the catalyst operating at the kinetic limit, i.e., the catalyst is
limited by reaction kinetics and not by the heat transfer (Fig. 5). This is
an important observation, as it is in stark contrast to the externally fired
case. Additionally, due to the improved activity of Cu⊂CoNi, 95%
conversion of methane to hydrogen was realized using roughly 15%
smaller applied magnetic fields as compared to CoNi for flows of 152
Nl h-1.
Figure 4. Field dependence of hysteresis heating per loop cycle for CoNi
obtained from hysteresis measurements performed at temperatures between
200C and 950C at the indicated values of Bmax. Error bars represent standard
deviations calculated for four consecutive runs. Solid lines are guides to the eyes.
(3)
푊H = ∮ 휎(퐵app) d퐵app
퐵
max
where 휎 [Am2·kg-1] is the specific magnetization (magnetic moment
per sample mass), indicates the heat generated per cycle in units of
J·kg-1 upon cycling the applied magnetic field between +Bmax to
The robustness of CoNi was evaluated in
a prolonged
experiment with a constant flow-rate of 101 Nl·h-1 with a feed gas
mixture of 29.7% CH4, 59.5% H2O and 10.8% H2 (mole %), an input
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case of externally fired SMR, highlighting the excellent heat transfer
from the induction field to the magnetic susceptor and active catalyst.
Combining chemically robust NPs with induction-heated
catalysis may prove useful for many other industrial reactions, as the
NPs can be modified to contain whatever active metal may be needed,
and the operating temperature controlled by adjusting the applied field.
The implementation of induction heating in SMR may eliminate
expensive waste-heat sections used in traditional methane reforming
setups, significantly reducing the complexity of the process design and
has the potential to drastically lower CO2 emissions from the
process.[28] This, together with the possibility of fast plant startup,
holds promise for these materials as competitors for classical hydrogen
plants or as part of ammonia plants in a future hydrogen economy and
especially for ad hoc small-scale demands.
Figure 6. Overview of prolonged reforming experiment on CoNi using the induction
heated setup mentioned earlier. The figure shows no loss of activity within the time
frame of the experiment. The bump observed at t = 72h is due to instrumental
instabilities (see full text). Inset figure shows the XRD diffractogram before and after
the experiment. A larger view may be found in Fig. S19.
Keywords: Heterogeneous catalysis • Hysteresis • Induction Heating •
Nanoparticles • Steam Reforming
temperature of 237C, at close to atmospheric pressure, under an
applied magnetic field of ca. 32 mT and a frequency of 69 kHz. Under
these conditions, the conversion of methane was 90-95%,
corresponding to an equilibrium temperature of 715C. In the time
frame of the experiment, which was >300 hours, no significant
decrease of the activity was observed as evidenced by the constant
value of the methane conversion (Fig. 6, red data points). The recorded
time interval (~14 days) is clearly much shorter than a typical reactor
lifetime (years), but on the other hand, it is the time interval where
most changes to the catalyst would be expected to occur. The drop
observed in CH4 conversion at 72 hours is a result of water
contamination of the gas chromatograph (GC) caused by a short power
outage and does not represent an actual loss of catalyst performance.
To avoid further damage, GC measurements after this point were
performed in steps, roughly 24 hours apart. The reactor outlet
temperature was measured constantly throughout the experiment (black
data points) using a Type-K thermocouple as described in the SI.
Subsequently, the catalyst was unloaded and checked for changes in
composition by XRD, ICP and STEM (Figs. 2, S19-S21). All of these
results underline the remarkable stability of the NP material, as no
structural changes were found in addition to no carbon formation and
no change of the Co wt.% ratio, which was practically unchanged at
51.8 wt.% (±2.0 wt.%) (Fig. 2).
In summary, the preparation of a new chemically tailored
nanostructured system was presented and its use in induction heated
SMR was demonstrated. The chemical synthesis of metallic NPs
allowed for the controlled production of a sample with a uniform and
predictable Ni-Co alloy composition. Compared to previous ideas,[25]
the realization of well-defined NPs through chemical synthesis led to
an increase in both hysteresis opening and steam reforming catalytic
activity, presumably caused by a larger fraction of the NPs being
ferromagnetic at the elevated reaction temperature. As a result, a
marked increase was found in the efficiency of the NPs in terms of
energy conversion under induction-heated steam reforming using only
a magnetic field generated from electrical current as a power source.
With similar or even slightly inferior magnetic properties, Cu⊂
CoNi demonstrated significantly improved reforming properties
compared to CoNi, opening up for the possibility of producing even
better catalysts by engineering the reactivity, as this is presently the
limiting factor. Finally, we show the stability of chemically
synthesized NPs to be excellent, and essentially inert to degradation in
the first 300 hours of operating at reforming conditions. Examining the
CH4 conversion under such conditions revealed that kinetic effects
alone and not thermodynamics hampered the catalyst, opposed to the
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COMMUNICATION
Layout 1:
COMMUNICATION
A well-defined alternative to traditional
steam reforming is presented herein. The
catalyst system, based on alloyed CoNi
nanoparticles is shown to be a very
capable candidate for induction-heated
catalysis. Dual functionality is observed
in the material acting as both catalyst
and magnetic susceptor, revealing
effective induction heating above 800 °C
Morten G. Vinum*, Mads R. Almind, Jakob
S. Engbæk, Søren B. Vendelbo, Mikkel F.
Hansen, Cathrine Frandsen, Jesper
Bendix, and Peter M. Mortensen*
Page No. – Page No.
A Dual Function Nanomaterial Tailored
for High-Temperature Induction-Heated
Catalysis
resulting
from
it’s
inherent
ferromagnetic nature.
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