Synthesis of Zinc Sulphide Nanoparticles
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1 Synthesis of Zinc Sulphide Nanoparticles The procedure shown here was adapted from an adaption by Paul Hansen and George Lisensky from Kurt Winkelmann, Thomas Noviello, and Steven Brooks, "Preparation of CdS Nanoparticles by First-Year Undergraduates," J. Chem. Educ. (2007) 84, , which was based on M. L. Curri, A. Agostiano, L. Manna, M. D. Monica, M. Catalano, L. Chiavarone, V. Spagnolo and M. Lugarà, J. Phys. Chem. B, (2000) 104, Preamble Zinc sulphide is a very important II VI semiconductor material with a wide direct band gap (E g = 3.68eV for bulk ZnS). It has been studied due to its wide applications as phosphors and catalysts as well as electro luminescent devices, solar cells and other opto electronic devices. ZnS is also of interest as small biomolecular probes for fluorescence and laser scanning microscopy. It is currently used as a shell or capping layer in nanoprobes such as CdSe/ZnS core structures. Aim You will use absorbance spectrum for bulk and nano sized ZnS particles, supplied to you, to calculate the diameter of the nanoparticles. Introduction Zinc sulphide can be made through the following chemical reaction: ZnCl 2 (aq) + Na 2 S(aq) (you need to complete the balanced chemical equation) In order to stop agglomeration of the nanoparticles formed and thus allow the formation of larger, non nanosized (bulk) particles we need is some type of nano sized reaction vessel. One in which the size of the vessel limits the growth of the sulphide particles. Micelles can be used to do this (refer to the lecture) The solvent is hexane an organic, hydrophobic liquid and small amounts of aqueous solutions are added. The charged end of the surfactant will be pointed towards the centre of the micelle and the nonpolar portion of the molecule will be exposed to the nonpolar solvent. Such a structure is called a reverse micelle. Figure 1 illustrates the difference between micelles and reverse micelles. (a) (b)
2 Figure 1. (a) micelle, (b) reverse or inverse micelle As the particle size is a function of micelle size, we could look at making different sized micelles. Hexadecyltrimethyl ammonium bromide or cetyltrimethyl ammonium bromide (CTAB) has a long hydrophobic chain and a polar head group. (Figure 2 (a)). The molecule does not dissolve well in either aqueous or organic solvents. In an organic solvent containing a small amount of water the hexadecyltrimethylammonium bromide traps the aqueous portion in a micelle sphere with the polar heads facing in and the non polar tails facing out ( as per Figure 1 (b)) Mixing hexadecyltrimethylammonium bromide pentanol micelles of ZnCl 2 with similar micelles containing Na 2 S produces nanoparticle ZnS since the aqueous solution serves as a nanoreactor and the particles cannot grow bigger than the micelle. The pentanol also acts as a capping agent to stabilize the ZnS particles. The formation of ZnS nanoparticles can be detected by spectroscopy since quantum size effects make the visible absorption spectra different than that of bulk ZnS. If we use different size surfactants, we should be able to produce different sized micelles. Use dodecyltrimethyl ammonium bromide (shorter tail) DTAB (Figure 2(b)) Dioctyl sodium sulfosuccinate (double tail) AOT (Figure 2(c)) (a) (b) (c) Figure 2. The surfactants a) CTAB, b) DTAB, c) AOT
3 Another way would be to use different amounts on pentanol. (See Figure 3). The relative amount of pentanol co surfactant controls the size of the micelle. More pentanol would make the diameter bigger. surfactant pentanol Figure 3. A water in oil microemulsion droplet. This static picture does not properly convey "the dynamic reality of the aggregates." Figure based on J. Phys. Chem. 100, (1996). Calculations The x intercept of the linear portion of the absorbance as a function of wavelength graph is a measure of E g. It can be shown that: Where is taken from the x intercept of the linear portion of the absorbance wavelength graph (absorbance edge bandwidth) When the absorbance spectra of ZnS particles of different size are measured it is found that there is a blue shift (towards a shorter wavelength) of the spectra as the particle size decreases. (Figure 4) This indicates a strong quantum size effect. This shift can be utilized in determining the crystal radius using the effective mass model of Yoffe (A.D Yoffe, Adv. Phys., 42, 172 (1993)) Figure 4. Effect of particle size on the absorbance spectra.
4 It can be shown that the absorbance edge of the nanoparticles is: where r is the radius of the nanoparticle. The part represents the reduced mass of electron hole effective mass, where m e * is the effective mass of the electron = 0.34m 0 and m h * is the effective mass of the electron hole = 0.23m 0. m o is the electron mass (9.106 x g). After multiplying by r 2, rearranging and using the quadratic formula, Where: e = 1.60x10-19 C (charge on electron) ε0 = 8.85x10-12 C 2 /N/m 2 (permittivity of free space) h = 6.63x10-34 J s (Plank s constant) c = 2.998x10 8 m/s for ZnS ε = 8.76 (relative permittivity) me* = 0.34mo = x kg mh* = 0.23mo = x kg (constants for ZnS from Borah, J.P. & Sarma, K.C. Acta Physica Polonica, 114, 4, pp , 2008) This can be simplified for our experiment to: Questions What is the band gap energy for each condition? Note that the energy values calculated above are in Joules. Use these for further calculations. o By convention, band gaps are usually quoted in electron volts. The conversion is simple:
5 1eV = x J What is the diameter of the ZnS nanoparticles for the CTAB + 1ml pentanol and the CTAB+ 0.5ml pentanol? Using these data and that provided in the table in the results section, describe why the structure of the surfactants give different diameters. Do the trends observe match what is to be expected? What properties would be affected by this change in band gap? What does this mean as far as producing a tunable material? Make general comments! Results 1 CTAB
6 0.3 CTAB Wavelength of absorption edge (nm) Pentanol (ml) CTAB DTAB AOT Bulk ZnS 342
7 Experimental Procedure ADDENDUM Note: The reagents have been tested by adding a drop of aqueous Zn 2+ to a drop of aqueous S 2. A bluey white colour should appear if the Na 2 S solution is good. If the mixture remains clear, remake the Na 2 S solution. Add 0.20 g of the surfactant, e.g. hexadecyltrimethylammonium bromide, to a test tube. The weight can be 0.19 to 0.21g, as long as it is in excess. Add 4.0 ml heptane and 1.0 ml pentanol to the surfactant. (Some groups may be directed to use 0.5 ml of pentanol instead). Stir to give a suspension. A vortex mixer is found to do this best. Press test tube into rubber cup to activate hold on tight! Immediately transfer half the suspension to a second tube. Stir both solutions to maintain the suspension. To one test tube, add 0.1 ml of M ZnCl 2. The solution will clear as hexadecyltrimethylammonium bromide micelles containing ZnCl 2 form. To the second test tube, add 0.1 ml of M Na 2 S. The solution will clear as hexadecyltrimethylammonium bromide micelles containing Na 2 S form. Join the two solutions and mix. The solution should go clear again. Record the UV absorption spectrum in a quartz cuvet. Note: Use a pentanol/heptane mixture of the same concentration as above in the reference cell. This removes the contribution of the solvents to the measured absorption spectrum. In a quartz cuvet, add an equal amount of aqueous M Zn 2+ and aqueous M S 2. Record your observations and immediately obtain the UV absorption spectrum (before the solution becomes too opaque). This is the bulk ZnS particle suspension. We shall attempt the last one. Repeat the experiment but, this time, add 0.5ml pentanol to 4.5ml of heptane. If we have time we will also try the other surfactants. We could try some different reactants. For example, instead of M ZnCl 2 add to one test tube, 0.05 ml of M ZnCl 2 and 0.05ml 0.012M MnCl 2 with both concentrations of pentanol/heptane mixtures.
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