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Photoassisted Hydrogen Production Using Visible Light and Coprecipitated Zinc Sulfide.Cntdot.Cadmium Sulfide Without a Noble Metal N

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Photoassisted Hydrogen Production Using Visible Light and Coprecipitated Zinc Sulfide.Cntdot.Cadmium Sulfide Without a Noble Metal N Subscriber access provided by University of Texas Libraries Photoassisted hydrogen production using visible light and coprecipitated zinc sulfide.cntdot.cadmium sulfide without a noble metal N. Kakuta, K. H. Park, M. F. Finlayson, A. Ueno, A. J. Bard, A. Campion, M. A. Fox, S. E. Webber, and J. M. White J. Phys. Chem., 1985, 89 (5), 732-734• DOI: 10.1021/j100251a002 • Publication Date (Web): 01 May 2002 Downloaded from http://pubs.acs.org on February 12, 2009 More About This Article The permalink http://dx.doi.org/10.1021/j100251a002 provides access to: • Links to articles and content related to this article • Copyright permission to reproduce figures and/or text from this article The Journal of Physical Chemistry is published by the American Chemical Society. 1155 Sixteenth Street N.W., Washington, DC 20036 732 J. Phys. Chem. 1985, 89, 132-134 ignored since transitions to them from the So ground state are not entirely inconsistent with experiment. allowed by the symmetry selection rules.23 The best-fit parameters The So potential is relatively flat near the minimum compared for So are V2= -3980.0 cm-' and V4 = -1023.0 cm-I, and those to that of a harmonic oscillator. This shape is required to re- for SI are V2= -2054.9 cm-I and V4 = -1009.2 cm-'. These same produce the negative anharmonicity in the So(a) spacings. The potential parameters were used to calculate the 9PA-dS torsional irregular positive anharmonicity in the Sl(A) spacings requires frequencies which appear in the last column of Table 11. Again, a double-minimum potential. The displacement of the equilibrium agreement is nearly within the experimental uncertainty. An geometry in SI compared to that in So correlates well with the independent fit of the 9PA-d5data gives the So potential param- observed maximum intensity of the A;f progression at n = 4. The eters V2 = -4209.2 cm-' and V, = -1094.4 cm-', and the SI Franck-Condon factors calculated for the best-fit potentials give parameters V, = -2465.2 cm-I and V4 = -1 122.2 cm-'. These an A;f peak at n = 5, in reasonably good agreement with exper- potentials, shown as dotted lines in Figure 3, differ by less than iment. A quantitative calculation of the line intensities for these about 10% from the potentials fitted to the 9PA data, which is transitions will require higher-order corrections to the simple probably less than the statistical uncertainty. Naturally, these Franck-Condon factors.23 potentials are to be regarded as valid only in the region near the In conclusion, it has been possible to determine the low-energy minima, in which the experimentally determined vibrational levels torsional potentials for 9PA in both So and S1 by analysis of the lie. The inclusion of V, potential terms results in only a slight free-jet LIF spectra. These potentials reproduce quantitatively improvement to the quality of the fits and negligible changes of the experimental So(a) and S,(A) transition frequencies in 9PA the potentials in the well regions. and 9PA-d5, and the calculated Franck-Condon factors are in The fitting procedure we have employed leads to an arbitrary qualitative agreement with the observed Sl(A) intensities. We phase factor of 90' in the So and SI torsional potentials. For- expect that 9PA, along with the other prototype molecules for tunately, it is possible to establish the actual position of the PO- which data on torsional vibrations is becoming available, will serve tential in terms of + by employing additional evidence. First of as a valuable point of reference for photochemical and photo- all, an examination of a space-filling molecular model for 9PA physical studies of molecules which exhibit large-amplitude vi- shows that the planar (+ = Oo) form is significantly destabilized brational motions. by severe periplanar repulsions between the ortho-hydrogen atoms on the phenyl ring and the nearest hydrogens of the anthracene Acknowledgment. The authors are indebted to Prof. Clayton moiety. We therefore assign the torsional minimum of So to 90°. F. Giese for providing the pulsed beam source used in these The phase of the SI torsional potential can be established (relative experiments and to Dr. Jaan Laane for giving us a copy of the to the So potential) by an analysis of the intensity pattern of the computer code22which we used to determine the torsional potential torsional transitions in Figure 2a. Franck-Condon factors cal- parameters. This research was supported by the National Science culated with the potentials as shown in Figure 3 are in good Foundation, Grant Nos. CHE-8205769 and CHE-8351158, and agreement with the observed intensities. In contrast, if the SI by the Graduate School of the University of Minnesota. potential is rotated by 90°, the predicted intensity pattern is Supplementary Material Available: Supplementary Material Available: Assignments of the 9PA and 9PA-d5 fluorescence (23) Herzberg, G. "Electronic Spectra and Electronic Structure of Poly- excitation spectrum, Tables I and I1 (6 pages). Ordering infor- atomic Molecules"; Van Nostrand-Reinhold: New York, 1966; Chapter 2. mation is given on any current masthead page. Photoassisted Hydrogen Production Using Visible Light and Copreclpitated ZnS.CdS without a Noble Metal N. Kakuta, K. H. Park, M. F. Finlayson, A. Ueno, A. J. Bard, A. Campion, M. A. Fox, S. E. Webber, and J. M. White* Department of Chemistry, University of Texas, Austin, Texas 78712 (Received: November 8, 1984) ZnS and CdS coprecipitated into Nafion films and onto Si02have been used for photoassisted catalysis of H2 production in aqueous sulfide solution. With visible light and no noble metal catalyst, the ZnS-CdS catalyst is as active for H2 generation as Pt/CdS. There is no major difference in activity of the Nafion- and silica-supported catalysts. Introduction corporated in Nafion membranes. It was shown that this system Hydrogen production from water using semiconductor photo- compared favorably with the best systems reported to date for catalysts has been actively studied in recent years.I4 In previous colloidal CdS dispersions. paper^,^,^ we reported the advantages, construction, and operation Mixed semiconductor systems offer potential advantages for of a photocatalyst system which consisted of platinized CdS in- solar energy utilization because of the possibilities presented by interparticle electron transfer' and special properties (tuning of (1) A. J. Bard, J. Phys. Chem., 86, 2 (1982). bandgap) of cofabricated systems.* In the present work, we report (2) J. M. White, "Photoassisted Reactions on Doped Metal Oxide our initial results for hydrogen generation in a supported (Nafion Particles" in 'Heterogeneous Atomospheric Chemistry", D. R. Schyrer, Ed., and silica) mixed semiconductor system, ZnSCdS, that does not American Geophysical Union, Washington, DC, 1983, Geophysical Mono- require a noble metal catalyst. For this system, hydrogen gen- graph 26, p 122. (3) M. Gratzel, Acc. Chem. Res., 14, 376 (1981). eration is comparable to Pt/CdS/Nafion6 and is much more (4) D. Meissner, R. Memming, and B. Kastening, Chem. Phys. Lett., 96, -.74 (19R(1\\-___ (5) K.'Krishnan, J. R. White, M. A. Fox, and A. J. Bard, J. Am. Chem. (7) N. Serpre, E. Borgarello, and M. Gratzel, J. Chem. SOC.,Chem. Soc., 105, 7002 (1983). Commun., 342 (1984). (6) A. W.-H. Mau, C.-B. Huang, N. Kakuta, A. J. Bard, A. Campion, J. (8) A. Henglein and M. Gutierrez, Ber. Bunsenges. Phys. Chem., 87, 852 M. White, and S. E. Webber, J. Am. Chem. Soc., 106, 6537 (1984). (1983). 0022-3654/85/2089-0732$01.50/0 0 1985 American Chemical Society Letters The Journal of Physical Chemistry, Vol. 89, No. 5, 1985 133 efficient than for either semiconductor alone. 0.06 Experimental Section A ZnS.CdS/Nafion Preparation. Prior to semiconductor in- corporation, Nafion 117 membranes were cleaned as described h v) earlier.6 Single-component systems were prepared by soaking in 0 either Cd(N03)2or Z~I(NO~)~solution (0.5 M) followed by 0 treatment with H2S. The mixed system was prepared by soaking F in an equimolar solution of ZII(NO~)~and Cd(N03)2(0.5 M -. each). Soaking times of greater than 5 min saturated the films. 5 0.04 C The soaking was followed by rinsing in distilled water to remove 0 .-* excess and unbound metal ions. The films were then immersed m in distilled water through which H2Swas bubbled for 10 min. The E films are denoted ZnS-CdS/Nafion, CdS/Nafion, or ZnS/Nafion, LL depending on their composition. cu The films were analyzed by X-ray powder diffraction (XRD). I No XRD signals of ZnS were observed for either the ZnS. 0.02 CdS/Nafion or the ZnS/Nafion. CdS/Nafion films, on the other hand, exhibited relatively strong XRD peaks corresponding to hexagonal CdS6 Although small peaks (presumably due to hexagonal CdS) were obtained for the mixed ZnS.CdS/Nafion system, the intensities were too weak to make a positive identi- fication. These results show that CdS crystal growth is influenced by coprecipitation of ZnS and that crystallite sizes are very small (<30 A). SEM of ZnS.CdS/Nafion showed a rough surface with particle sizes on the order of 0.5 pm. 0 1 2 3 456 The films (1 X 1 cm when dry) were immersed in Pyrex glass Time (hours) cells containing 3 mL of 0.1 M Na2S. The vessels were degassed under vacuum with sonication to remove gases from the interior Figure 1. Photogeneration of H2 from Pt/CdS/Nafion (curve A) and of the membrane and were purged with N2 Then the vessels were ZnS.CdS/Nafion (curve B) films by visible light (A > 440 nm).
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