i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 3 5 ( 2 0 1 0 ) 7 8 2 7 e7 8 3 4

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Synthesis and characterization of layered FePS3 for

hydrogen uptake

N. Ismail a,*, A.A. El-Meligi a, Y.M. Temerk b, M. Madian a

a
National Research Center, Physical Chemistry Department, Center of Excellence for Advanced Science, Renewable Energy Group, Cairo,
Egypt
b
Assiut University, Faculty of Science, Chemistry Department, Assuit, Egypt

article info abstract

Article history: Iron phosphorus trisulfide FePS3 is related to the chalcogenides. It is characterized by
Received 16 January 2010 layered structure. FePS3 powder was prepared by solid state reaction and heated up to
Received in revised form 650
C using two different heating rates 1
C/min and 40
C/min. The results showed that
2 May 2010 the FePS3 produced with slow heating rate was highly ordered single crystalline phase
Accepted 12 May 2010 while the powder produced with the fast heating rate was poly crystalline phase. The
Available online 17 June 2010 surface morphology and the grain size were influenced by the heating rate used for
preparation. The thermal resistance of the highly ordered crystalline phase extended till
Keywords: 680
C while the less ordered one extended to 660
C. The products at 900
C revealed
Metal phosphorous trisulfide partial decomposition of FePS3 with subsequent formation of iron sulfide phases poorer
Hydrogen sorption with sulfur element. The FePS3 of single crystalline phase exhibited higher hydrogen
Layered material sorption capacity at different temperatures than the less ordered crystalline phase.
Hydrogen capacity was reduced by cycling as the interlayer gap shrinks.
ª 2010 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.

1. Introduction metal chalcogenides MPX3 (M^first row transition metals;

Research over the last decade focused on chemical and phys-
ical hydrogen storage based materials poses possible mecha-
nisms for reversible storage. Plenty of materials are tested,
among them, metal hydrides light and complex [1], nitrides-
imides-amides [2e5], multicomponent systems [6], zeolites [7]
and recently metal organic frameworks (MOFs) [8,9]. Never-
theless, intensive efforts have been pushed to meet the prac-
tical demands required of a solid state storage system, namely
high storage density together with favorable sorption ther-
modynamics and kinetics and prolonged cycle ability and
lifetime, significant challenges remain keeping safe, efficient
hydrogen storage far from mobile application concerns [10,11].
Materials with layered structure attract attention because
of two dimensional structure features. It gives rise to strong
anisotropies in the physical properties [12e15]. Transition
X^S or Se) show fascinating structure, electric and
magnetic properties [16e18]. The unit cell containing
a group Fe2P2S6 is shown in Fig. 1 [19], where hexagonal
sulfur sheets are arranged along the c axis in an ABCABC
stacking planes. The “Van der Waals” weak bonded empty
gaps between planes are easily intercalated by molecules or
ions either by the reduction of the host or substitution of
the metal cations [20,21]. This adds interesting feature to
these compounds is their application as cathode materials
for rechargeable high-energy-density lithium batteries
[22,23]. As a consequence of intercalation is the increase in
the layer spacing due to the insertion of guest material into
the “Van der Waals” gap.
Our idea is based on using the “Van der Waals” gap to
occupy hydrogen and to evaluate the FePS3 as a hydrogen
storage material.

* Corresponding author. Fax: þ20 233370931.

E-mail address: nahlaismail24@yahoo.com (N. Ismail).
0360-3199/$ e see front matter ª 2010 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.ijhydene.2010.05.061
7828 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 3 5 ( 2 0 1 0 ) 7 8 2 7 e7 8 3 4

were mixed thoroughly. The mixed brown powders were

sealed in two silica ampoules under vacuum of 102 bar.
These ampoules were put in a programmable heating rate
S2 furnace. The first ampoule was heated from room tempera-
ture to 650
C using 40
C/min heating rate. The temperature
S5 S4
was then remained at 650
C for 6 days [24]. The other
ampoule followed the same experimental sequence using
a heating rate 1
C/min. Then the silica ampoules were left to
P2 cool inside the furnace till room temperature. The ampoules
were broken and the synthesized FePS3 black powders were
M1 ground.
This is the first time to study the preparation of MPS3
S3 S1 compounds with different heating rates and its influence on
the material structure.
In this article, we point out to sample prepared using
S6 40
C/min heating rate as sample (A) and the sample
prepared by 1
C/min as sample (B).
M2
Fig. 1 e The unit cell of FePS3 where M^Fe.
2.2. Techniques

Powder X-ray diffractograms (XRDs) were recorded in the

In this work we propose new family Transition metal
chalcogenides, not suggested before, to the field of hydrogen
storage. To our knowledge this class of materials is not
studied before for the purpose of hydrogen energy storage.
FePS3 is not expensive and its preparation is feasible.
2. Experimental methods
2.1. Synthesis
Two black samples of powder FePS3 compound were prepared
by solid state reaction between stoichiometric amounts of the
elemental powders, Fe, P and S of purity 99.98%. The elements
range 5
< 2q > 70
, and time 2 s per step with Philips X0 pert
instrument of CuKa radiation (l ¼ 1.5418  A)
The IR spectrum of the powder was recorded in KBr disks
containing a small amount of the compound, with a JASCO FT/
IR 6300.
The thermal stability of the prepared materials and its
decomposition temperature were determined from its ther-
mogravimetric analysis (TGA) curves for 10 mg of the black
powder by an apparatus “DSC Q 600”-V 20.5 under nitrogen
flow atmosphere using a heating rate 10
C/min.
Surface morphology of FePS3 powder was studied by
scanning electron microscopy (SEM) JEOL JXA-840A. The
powder was spread over double face scotch tapes attached to
the holder and sputtered with gold. The voltage used was
30 kV and the magnification was 3500.

(001)
Intensity (a.u.)

(b)

(a)

5 10 15 20 25 30 35 40 45 50 55 60 65 70

2 deg. )

Fig. 2 e XRD patterns of FePS3 powder, (a) sample A as-prepared (b) sample B as-prepared.
 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 3 5 ( 2 0 1 0 ) 7 8 2 7 e7 8 3 4 7829

Fig. 3 e The Atomic building of FePS3.

The transmission electron microscopy (TEM) experiments

were carried out at room temperature, on JEOL-1230 micro-
scope running at 120 kV with a tungsten cathode. The sample
was prepared by adding minute amount of the powder to de-
ionized water. Then ultra-sonication was performed to obtain
a suspension of thin particles. One droplet of this dispersion
was deposited on a holey carbon grid and after evaporation of
water, the particles stuck to the carbon film.
The specific surface area (SBET), the total pore volume (Vp)
and the mean pore radius (r) of various adsorbents were
determined from nitrogen adsorption isotherms measured at
196
C using NOVA automated gas sorbometer. The values of
Vp were computed using the relation

Vp ¼ 15:45  104  Vst cm3 =g (1)

where Vst is the volume of nitrogen adsorbed at P/P tends to
unity. The values of r were determined from equation (2) Fig. 5 e SEM images of FePS3 (a) sample A; (b) sample B.

2Vp
r ¼ 104 
A (2)
SBET
a volumetric method using an AMC PCI-HP 1200 equipment.
The determination of hydrogen content was carried out by the
Temperature was controlled with a precision of 0.1
C. The
measurement of pressure-composition isotherms (PCI) by
accuracy of hydrogen content measurements was 0.04 wt%.
In order to minimize contamination from air the compound
powder was degassed at 200
C for 1 h under dynamic vacuum
before test. Pressure-composition isothermal (PCI) plots were
traced under the above mentioned conditions. In addition, the
sorption kinetics at 193
C was evaluated.

(a) 3. Results and discussion

Intensity (a.u.)

(b)
3.1. X-ray powder diffraction (XRD)

The structure of the prepared samples A and B is identified by

441
X-ray diffractograms shown in Fig. 2(A) and (B). All charac-
teristic diffraction lines of the FePS3 phase are observed,
indicating the formation of the compound. The sharpness of
570 the different peaks suggests the formation of big size crystals
of FePS3 of [001] line reflection [25]. The peak area of Sample B
1000 950 900 850 800 750 700 650 600 550 500 450 400
is nearly five-fold sample A. The main peak of sample A is
shifted to lower Bragg’s angle (2q) than sample B so that, the
Fig. 4 e IR spectra of FePS3, (a) sample A as-prepared (b) main peak of sample A lies at 2q ¼ 13.87 and d spacing equals
sample B as-prepared. 6.37 while the main peak of sample B lies at 2q ¼ 13.77 and
7830 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 3 5 ( 2 0 1 0 ) 7 8 2 7 e7 8 3 4

Fig. 6 e TEM images of FePS3 powder; (a) particle dispersion (b), (c) and (d) of sample B; (e) and (f) of sample A; (g),(h) Electron
diffraction pattern of samples B and A respectively.

d spacing equals 6.42. It is deduced that the slow heating rate
during preparation enhances well crystalline ordered phase
and widen the interlayer distances.
According to standard 1998- JCPDS card 78-0496, the XRD
patterns are indexed in the monoclinic unit cell space group C2/
m in which the calculated parameters by a least-squares refine-
ment of the observed reflections, are a ¼ 5.947 
A, b ¼ 10.300 
A,


c ¼ 6.7222 A, and b ¼ 107.16 . The atomic building of the FePS3
layers is shown in Fig. 3. It has been performed using “Atoms”
software program, as explained in previous literature [24].
 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 3 5 ( 2 0 1 0 ) 7 8 2 7 e7 8 3 4 7831

100 3.3. SEM and TEM investigations

95 Sample B
Sample A
Scanning electron microscopy images taken to A and B
90
samples are revealed in Fig. 5(A) and (B). Comparison between
85
both images from the first blink shows a significant difference
weight, %

80 in surface morphology. The heating rate during synthesis

75 plays role in the surface architecture and size. The relatively
70 fast heating rate (40
C/min) enhances the formation of thin
65
transparent agglomerated platelets. On the other hand, the
slow heating rate (1
C/min) in image (b), gives rise to coarse
60
undefined separated shapes, the lateral direction in some of
55
them looks like compact layers as it is marked by the arrows in
50 the image. The grain size in image (b) varies from 9 to 18 mm
100 200 300 400 500 600 700 800 900 1000
while its thickness varies from 0.6 to 1 mm. The slow heating
Temperature, °C rate induces the formation of coarse grains.
Fig. 7 e Thermogravimetric plots of FePS3. TEM images of FePS3 powders are shown in Fig. 6. Image (a)
informs homogeneous dispersion of particles. The images of
sample B are shown in (b), (c) and (d), and the images of the
The crystal size values estimated from XRD patterns for
sample A are provided by (e) and (f). Image (b) shows the
different types of iron phosphorus trisulfide samples were
formation of planes located over each other. In another loca-
obtained using Scherrer method [26] relating the crystallite
tion in the same sample, image (c) and (d) clearly show the
size to peak broadening introduced in equation (3).
formation of branched chains formed from regular spheres
d ¼ Klb1=2 cosq (3) almost the same size. Image (e) views the formation of layered
platelet clusters while image (f) views the formation of the
The crystal sizes of sample A of the three main peaks are branched chain formed from spheres. The particle size esti-
106.7, 79.5 and 90.02 nm respectively, The crystal sizes of mated for the regular spheres in sample A is 18e20 nm,
sample B are 133, 111.2 and 136.4 nm respectively. sample B shows coarser particle size than sample A of
It is clear that using heating rate 1
C/min in preparation of 30e65 nm. One may conclude that the relatively fast heating
FePS3 leads to increase the crystallite size. rate of the preparation is twilling the particle size.
The electron diffraction pattern in image (g) for sample B
3.2. Infrared spectroscopy (IR) confirms the preparation of a single crystalline phase (001)
FePS3. While the fast heating rate (Sample A) enduces the
The IR spectrum of pure FePS3 samples A and B (see Fig. 4(A) formation of poly crystalline phase as shown in image (h).
and (B) respectively) show the presence of the n(PS3)2
asymmetric stretching band at 570 cm1. This band is char- 3.4. Thermal resistance
acteristic for phosphorous trisulfide transition metal
compound [27]. Additionally, in the medium infra red band at Thermogravimetric analysis (TGA) curves of A and B are
441 cm1 a peak appears that corresponds to the y(PeP) bands introduced in Fig. 7. A slight weight loss of about 5 wt%
0
or T z(PS3). These studies confirm the formation of the desired appears at 200
C in sample A. Probably this is due to some
species. humidity present in the sample. The onset decomposition

Fig. 8 e XRD pattern of FePS3 at 900
C.

7832 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 3 5 ( 2 0 1 0 ) 7 8 2 7 e7 8 3 4

2.0
2.2
Sample B at -193 C
2.0 Sample A at -193 C 1.8 Sample A at -193 °C
1.8 1.6
Hydrogen content (wt%)

Hydrogen content (wt%)

1.6 1.4
1.4
1.2
1.2
1.0
1.0 Cycle1
0.8 Cycle2
0.8
Cycle3
0.6
0.6 Cycle4
0.4 0.4 Cycle5

0.2 0.2
0.0
0.0
0 2 4 6 8 10 12 14 16 18 20
0 2 4 6 8 10 12 14 16 18 20
Hydrogen pressure (bar) pressure (bar)
Fig. 9 e PCI curves of FePS3 sample A and B performed at Fig. 11 e PCI isotherms at L193
C of FePS3 prepared with
L193
C. fast heating rate.

temperatures of sample A and sample B are 660
C and 680
C
respectively followed by abrupt decrease of weight that ends
almost at the temperatures 765
C and 785
C respectively. The
total amount of weight loss at these temperatures is about
45%. Conclusion may be driven out from these results that the
preparation with relatively slow heating rate results in
formation of single crystalline phase, which improves the
thermal resistance of FePS3 powder so that the onset and the
final decomposition temperatures are shifted to higher
temperature values.
In order to figure out the change occurred that causes the
abrupt decrease in weight, the products of sample A and B
after thermal analysis till 900
C were X-rayed and the
diffraction patterns of both samples are similar and displayed
in Fig. 8. This pattern reveals that partial decomposition of
FePS3 occurred and the decomposition products are Fe7S8 as
minor compound and FeS2 as trace existing compound beside
the FePS3 as the major existing compound. The abrupt
decrease in weight shown in Fig. 7 could be due to the release
of sublimated sulfur during the partial decomposition of FePS3
with subsequent formation of iron sulfide phase(s) relatively
poorer with sulfur element.
3.5. Hydrogen storage characteristics of FePS3
The hydrogen sorption isotherm curves of FePS3 powder at
193
C are recorded in Fig. 9. Up to 20 bar, the isotherm shows
a linear progression over the investigated pressure range. The
hydrogen adsorption content reaches 2.2 wt% in sample B of
single crystalline phase and 1.7 wt% in sample A of poly
crystalline phase. Most probably molecular hydrogen is
adsorbed within the interplaner gap of Van der Waals forces
that may induce hydrogen adsorption within. More studies
were performed at different temperatures. At room tempera-
ture (25
C) and up to 20 bar hydrogen pressure, sample A and
B were able to store minute amounts of hydrogen 0.1 wt% and
0.2 wt% respectively. Decreasing the temperature till 100
C,

2.2
0.6
2.0 Sample B at -193 °C
-100 °C
0.5 1.8
Sample A
Hydrogen content (wt%)
Hydrogen content wt%

1.6
Sample B
0.4 1.4
1.2
0.3
1.0 Cycle1
0.8 Cycle2
0.2 Cycle3
0.6 Cycle4
0.4 Cycle5
0.1
0.2

0.0 0.0
0 2 4 6 8 10 12 14 16 18 20 0 2 4 6 8 10 12 14 16 18 20
Hydrogen pressure (bar) Pressure (bar)

Fig. 10 e PCI curves of FePS3 sample A and B performed Fig. 12 e PCI cycles of FePS3 prepared with slow heating
at L100
C. rate performed at L193
C.
 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 3 5 ( 2 0 1 0 ) 7 8 2 7 e7 8 3 4
3.2
3.0
2.8
2.6
2.4
Hydrogen content, wt%
2.2
2.0
1.8
1.6
-193 °C
1.4
1.2
1.0
0.8
0.6
0.4
0.2
0.0
0 10 20 30 40 50
time, min
Fig. 13 e The rate of hydrogen adsorption (solid symbol)
and its desorption (hallow symbol) of sample B at (a) 30 bar;
(b) 20 bar.
the amount of molecular hydrogen adsorbed reached 0.35 wt%
for sample A, and 0.6 wt% for sample B up to the same
hydrogen pressure. Fig. 10 displays the isotherms at 100
C.
Quite obvious that the single crystalline phase of relatively
wider d spacing distance is able to uptake more hydrogen in
the interlayer space distance at varies temperatures than the
polyscrystalline phase.
The specific surface area and the apparent micropore
volume were calculated from the physisorption isotherm data
of N2 at 196
C on the basis of BrunauereEmmetteTeller
(BET) theory [28]. BET analysis for sample B has specific
surface area (60 m2/g), the apparent micropore volume
obtained is 19  103 cc/g and the mean pore radius is 6.3 
A. On
the other hand, Sample A yields a relative smaller specific
surface area and less micropore volume so that the specific
surface area is 28 m2/g, the apparent micropore volume
obtained is 8  103 cc/g, and the mean pore radius is 5.7  A.
These results are in agreement with the hydrogen sorption
capacities as the increase in surface area and pore volume
should increase the physically adsorbed hydrogen.
In order to study the efficiency of hydrogen cycling, five
adsorption/desorption cycles were performed at 193
C and
up to 20 bar for both samples A and B. The results are dis-
played in Fig. 11 and 12. After each adsorption isotherm, the
powder undergoes full desorption. In both samples, cycling
reduces the hydrogen capacity by increasing the cycle
number, in a way that the hydrogen capacity of the fifth cycle
of sample A has been reduced by 17% while that of sample B
has been reduced by 9%.
The samples after cycling exhibit the same XRD patterns as
in Fig. 2 but the estimated d spacing values were lower so that
in sample A the d spacing became 6.3 and in sample B became
6.38. The slight decrease in the interlayer gap distance by
desorption may be the reason of the observed reduction in the
amount of hydrogen adsorbed by hydrogen cycling.
The IR spectra of the samples after hydrogen cycling did
not trace any change in sample A and B compared with the as-
prepared samples.
7833
(a) The rate of hydrogen adsorption is studied for sample B at
193
C and presented in Fig. 13. At 20 bar, the powder adsorbs
2.2 wt% within 30 min but the desorption rate is rather slow so
that it desorbs this amount of hydrogen thoroughly within
(b) 75 min. At 30 bar, the powder adsorbs 3 wt% of hydrogen
within 30 min then it continues to adsorb more hydrogen with
slow rate. At 85 min the sample adsorbs about 3.2 wt%. Its
desorption rate is similar to the desorption rate of the 20 bar
but till 90 min. The powder does not undergo full desorption
and about 0.1 wt% hydrogen remains in it.
4. Conclusion
60 70 80 90
Preparation of FePS3 layered material with different heating
rates has influenced the crystallinity of the product as well as
the interplanar gap in a way that slow heating rate results in
better well ordered single crystalline phase and wider inter-
planar space. This advantage allows the powder to store more
hydrogen in its interplanar space. Yet, hydrogen cycling is
reduced by increasing the number of cycles because the
interlayer distance shrinks.
To our knowledge this is the first time to examine FePS3 for
hydrogen sorption and to study the preparation with different
heating rates.
Acknowledgments
N. Ismail, A. A. El-Meligi and M. Madian are deeply grateful to
Prof. Hany El-Nazer and Prof. Nihad El-Chazly for their
administrative support. The Egyptian Science and Technology
Development Fund (STDF) is acknowledged for funding this
work.
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