Hydrogenation in SWCNTs Functionalized with Borane

D. Silambarasan*, V. Vasu, V. J. Surya and K. Iyakutti

School of Physics, Madurai Kamaraj University, Madurai-625021, Tamilnadu, India.

simbuphysics@yahoo.com

Abstract. We have done the experimental investigation of hydrogen storage in functionalized single-walled carbon
nanotubes (SWCNTs). The SWCNTs having the average diameter of 22 nm are deposited on alumina substrates by drop
casting method. The functionalization of SWCNTs with BH3 using LiBH4 as the precursor, over the surface of SWCNTs
is done by the same chemical method. Further, the functionalized samples are hydrogenated in the hydrogenation
chamber. The samples are characterized through FTIR, XPS and CHNS studies. A hydrogen storage capacity of 0.87 wt
% at 100º C is observed.
Keywords: Carbon nanotubes, Functionalization, Hydrogen storage.
PACS: 88.30.rh, 88.30.R-

INTRODUCTION the substrates. Then the substrates are heated to 275ºC

(decomposition temperature of LiBH4: which yield
The lacking and harmfulness of fossil fuels leads to diborane and d hydrogen) for 1h.
the consideration of hydrogen as the potential
alternative for energy services. The high RESULTS AND DISCUSSION
surface/volume ratio of nanomaterials has significant
implications with respect to energy storage. Figure 1 shows that the scanning electron
Functionalized single walled carbon nanotubes microscopy (SEM) images of purchased SWCNT, the
(SWCNTs) are one of the most promising materials, average diameter of SWCNTs are estimated to be 22
can adsorb and release a large quantity of hydrogen nm. Figures 2 and 3 shows the FTIR spectrum of
easily, reliably, safely and efficiently [1]. We have SWCNT coated on alumina substrates and SWCNT
done experimental investigation of hydrogen storage in functionalized with LiBH4 respectively. Peaks at 1575
functionalized SWCNTs. cm-1, 1631cm-1 are due to C=C stretching and isolated
stretching modes of vibrations respectively. A peak at
EXPERIMENTAL 1402 cm-1 is due to C-H deformation vibration. The
higher the BH3 dispersion higher is its reactivity with
Single walled CNTs with 2-propanol are taken in SWCNT. If the stretching bonds corresponding to
the ratio of 5 mg/ml and it is sonicated for 1 h to allow BH3/CNT are more then naturally the reactivity of BH3
the CNTs to be dispersed uniformly. The dispersed and CNT is more. In addition to the above said peaks
solution is then deposited drop wise on the alumina (Fig. 2), the new absorption peak (Fig. 3) at 2355 cm-1
substrates (19mm 19mm 0.65mm) maintained in air
~ 60°C using a micro pipette (alumina substrate was
taken as it will not react during a heating process).
After deposition, the sample is heated to 300°C for 1 h
to remove the impurities. Then the SWCNTs are
functionalized with BH3 using LiBH4 as the precursor.
Functionalization of CNT with BH3 enhances the
binding energy of hydrogen molecules as well as
increases the storage capacity [2].Lithium borohydride
LiBH4, yields diborane on heating [3]. LiBH4 with Di
ethyl ether were taken in the ratio of 25 mg/ml and it is
drop casted over the surface of SWCNT deposited on FIGURE 1. SEM image of SWCNT.
Solid State Physics, Proceedings of the 55th DAE Solid State Physics Symposium 2010
AIP Conf. Proc. 1349, 291-292 (2011); doi: 10.1063/1.3605849
© 2011 American Institute of Physics 978-0-7354-0905-7/$30.00

291

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 FIGURE 5. XPS of C, B.
FIGURE 2. FTIR Spectrum of SWCNTs.
Hydrogenation
The weight percentage of the hydrogen content in
functionalized samples is 0.006 wt%. The samples are
hydrogenated at 100 ºC for 20 min at a flow rate of 1
liter/min. After, hydrogenation the hydrogen content of
about 0.873 wt% was observed. Therefore, the
hydrogen content of the samples has increased by
0.867 wt%. Trials are being carried out to improve the
storage capacity by varying the hydrogenation
FIGURE 3. FTIR Spectrum of functionalized SWCNTs. conditions.

occurs due to asymmetric B-H stretching in Borane B- CONCLUSION

H3 complexes, the peaks at 2387 and 1182 cm-1 are
due to stretching and bending mode of B-H bond in the The SWCNTs with average diameter of 22 nm
BH3 group respectively [4, 5]. The presence of BH3 in deposited on alumina substrates have been
the functionalized sample is confirmed by this FTIR successfully functionalized with BH3. A hydrogen
study. The absorption peak corresponding to C-H storage capacity of 0.87 wt% is achieved at 100º C.
bond is observed at 3080 cm-1. Our experimental result
reveals that there is a bond between one of the
hydrogen in BH3 and carbon in the SWCNTs. Also X-
ACKNOWLEDGMENTS
ray photoelectron spectroscopy study is carried out to
find the other possible elements present in the sample. The authors thank Asian Office of Aerospace
Research and Development (No. 09-4157), USRF-
The full survey spectrum of our sample is shown in
MKU, UPE and CSIR.
Fig. 4. The C 1s and B 1s regions of the XPS spectra
are displayed individually in Fig. 5. The C 1s
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FIGURE 4. XPS survey spectrum.

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