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First Paper
First Paper
First Paper
We describe for the first time the use of a single source precursor
to deposit thin films and nanocrystals of palladium selenide.
Fig. 2 pXRD pattern of as-deposited thin films of palladium selenide Fig. 5 I–V characteristic of PdSe films deposited at 500 1C.
Pd17Se15 (ICDD: 00-029-1437) at (a) 400 1C (b) 4501C and (c) 5001C. (ICDD 01-072-1197) and Pd17Se15 (ICDD 00-029-1437)
nanoparticles with the PdSe2 phase clearly dominant in OA
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deposition of palladium selenide thin films or nanoparticles. 10 ml of oleylamine was heated to 230 1C under nitrogen in a three neck
Thin films show the deposition of a single phase of palladesite flask for 1 h. The colour of the mixture changed to red-brown. After
cooling the flask to room temperature and addition of 20 ml of acetone
phase (Pd17Se15) at all growth temperatures. The solution into the flask gave a brown-black precipitate which was separated by
thermolysis carried out in oleylamine gave predominantly centrifugation.
PdSe2 with some Pd17Se15 whereas nanoparticles grown from
1 L. Y. Chiang, J. W. Sioirczeweki, R. Kastrup, C. S. Hsu and
DDSH or 1 : 1 mixture of DDSH and OA gave only Pd17Se15. R. B. Upasani, J. Am. Chem. Soc., 1991, 113, 6574.
The shape and size of nanoparticles was strongly dependent 2 S. Eijsbouts, V. H. J. DeBeer and R. Prins, J. Catal., 1988, 109,
upon the solvent system. 217.
3 S. Dey and V. K. Jain, Platinum Met. Rev., 2004, 48, 16.
Notes and references 4 H. Kyama and T. Iwata, Japanese Patent 08/095, 209, Mitsubishi
Paper Mills Ltd, 1996O. Tanabe, U.S. Patent 5,030,545, Fuji
y All the reactions were performed under nitrogen atmosphere by Photo Film Co Ltd, 1991.
using standard Schlenk techniques. All chemicals were bought from 5 S. Geller, Acta Crystallogr., 1962, 15, 713.
Published on 07 December 2010 on http://pubs.rsc.org | doi:10.1039/C0CC03079A
Sigma-Aldrich. NMR spectra were obtained on CDCl3 using a Bruker 6 T. Olsen, E. Roest and F. Groenvolt, Acta Chem., Scand. Ser. A,
AC300 FTNMR instrument. Element analysis was performed by The 1979, 33, 251.
University of Manchester micro-analytical laboratory. Single crystal 7 A. Singhal, V. K. Jain, R. Mishra and B. Varghese, J. Mater.
X-ray crystallography measurements were made using graphite mono- Chem., 2000, 10, 1121; B. Liladhar, J. V. Jain, P. P. Phadnis and
chromated Mo-Ka radiation on a Bruker APEX diffractometer. The M. Nethaji, J. Organomet. Chem., 2007, 692, 1546; S. Dey,
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structures were solved by direct methods and refined by full-matrix V. K. Jain and B. Varghese, J. Organomet. Chem., 2001, 623, 48;
least-squares on F215 Mo-Ka radiation (l = 0.71073 Å). All non-H S. Dey, V. K. Jain, S. Chaudhury, A. Knoedler, F. Lissner and
atoms were refined anisotropically. H atoms were placed in calculated W. Kaim, J. Chem. Soc., Dalton Trans., 2001, 723; S. Dey,
positions by assigned isotropic thermal parameters and allowed to ride V. K. Jain, J. Singh, V. Trehan, K. K. Bhasin and B. Varghese,
on their parent carbon atoms. All calculations were carried out by Eur. J. Inorg. Chem., 2003, 744; B. Liladhar, K. J. Vimal and
using the SHELXTL package.16 CCDC 773721 (1). N,N diethyl-N 0 - B. Varghese, Inorg. Chim. Acta, 2006, 359, 409.
naphthoylselenourea (1): the preparation of the ligand (1) and its lead 8 S. Dey, S. Narayan, A. Singhal and V. K. Jain, Proc.-Indian Acad.
complex (2) was carried out by a modification of the method reported Sci., Chem. Sci., 2000, 112, 187; V. K. Jain, B. Liladhar, S. Dey and
in the literature.13,14 Instead of selenourea being isolated by addition N. D. Ghavale, Phosphorus, Sulfur Silicon Relat. Elem., 2008, 183,
of excess of water we used diethyl ether to extract selenourea. Yield, 1003; B. Liladhar, J. K. Vimal, P. P. Phadnis and M. Nethaji,
33%; elemental analysis (found: C, 57.6; H, 5.3; N, 8.3%, calc: C, 57.0; J. Organomet. Chem., 2007, 692, 1546; B. Liladhar, W. P Amey,
H, 5.4; N, 8.4%) IR: 3023 n(C–H), 1753 n(CQO), 1198 n(CQSe), 1361 J. K. Vimal, K. Siddharth and M. Nethaji, J. Organomet. Chem.,
n(C–N) cm1. 1H NMR (d CDCl3, 400 MHz) (400 MHz; CDCl3): 1.42 2009, 694, 3892.
(t, 3H), 1.30 (t, 3H), 3.6 (q, 2H), 4.18 (q, 2H), 7.85(m, Ar-4H), 7.56 9 J. Xuchuan, M. Brian, W. Yuliang, C. Bryan and X. Younan,
(p, Ar-3H), 8.5 (s, NH), mass (ES, negative scan) m/z 333 (100%), Chem. Phys. Lett., 2004, 385, 472.
ligand. [bis(N,N-Diethyl-N 0 -naphthoylselenoureato)palladium(II)] (2) 10 M. A. Malik, N. Revaprasadu and P. O’Brien, J. Mater.Chem.,
yield 54%, elemental analysis (found: C 48.30, H 4.0, N 7.0, Pd 2002, 12, 92.
14.6%). Calculated: C 50.0, H 4.2, N 7.3, Pd 13.8%. IR: 2977 11 I. B. Douglass, J. Am. Chem. Soc., 1937, 59, 740; I. B. Douglass
n(C–H), 1505 n(CQO, coordinated with metal), 914 n(CQSe, and F. B. Dains, J. Am. Chem. Soc., 1934, 56, 1408.
coordinated with metal), 1361 n(C–N) cm1. 1H NMR (d, CDCl3, 12 J. C. Bruce and K. R. Koch, Acta Crystallogr., Sect. C: Cryst.
400 MHz) (400 MHz; CDCl3): 0.74 (d, 12H), 0.87 (d, 12H), 1.6 (t, 2H), Struct. Commun., 2008, 64, m1; J. Dillen, M. G. Woldu and
2.1 (t, 2H), 3.5 (d, 4H), 3.78 (d, 4H), 8.28(m, Ar-8H), (APCI, K. R. Koch, Acta Crystallogr., Sect. E: Struct. Rep. Online,
acetonitrile) m/z 255(100%) binaphthyl. Crystal data for the ligand: 2006, 62, 05228.
Mr = 333.28, crystal system triclinic, space group, P1 a = 11.1943(8) Å, 13 J. Dillen, M. G. Woldu and K. R. Koch, Acta Crystallogr., Sect.
b = 11.2670(8) Å, c = 13.5411(10) Å, a = 72.631, b = 85.291, E: Struct. Rep. Online, 2006, 62, 04819; W. Bensch and
g = 66.501. Volume 1493.47(19) Å3, Z = 4, calculated density = M. Schuster, Z. Anorg. Allg. Chem., 1994, 620, 1479.
1.482 mg m3. AACVD deposition: AACVD experiments were carried 14 G. Horley, M. Lazell and P. O’Brien, Chem. Vap. Deposition, 1996,
out at deposition temperatures of 400–500 1C with an argon flow rate of 2, 242.
160 sccm for 1 h under atmospheric pressure. The reactor was 15 G. M. Sheldrick, SHELXL 97 and SHELXS 97, University of
purged with argon for 10 min at the required deposition temperature Gottingen, Germany, 1997.
before carrying out deposition in order to avoid any in situ oxidation. 16 SHELTXTL Version 6.10, Bruker AXS Inc., Madison, Wisconsin,
Synthesis of nanoparticles: 0.25g (0.32 mmol) of precursor (2) in USA, 2000.