synthesis of hybrid au–zno nanoparticles using a one pot polyol process

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Materials Chemistry and Physics xxx (2014) 1e8

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Materials Chemistry and Physics

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Synthesis of hybrid AueZnO nanoparticles using a one pot polyolprocess

Amine Mezni a, b, Adnen Mlayah b, Virginie Serin b, Leila Samia Smiri a, *

a Unit�e de recherche “Synth�ese et Structure de Nanomat�eriaux” UR11ES30, Facult�e des Sciences de Bizerte, Universit�e de Carthage, 7021 Jarzouna, Tunisiab Centre d'Elaboration de Mat�eriaux et d'Etudes Structurales, CNRS, UPR 8011, Universit�e de Toulouse, 29 Rue Jeanne Marvig, 31055 Toulouse, France

h i g h l i g h t s

* Corresponding author.E-mail address: [email protected] (L.S. Smiri).

http://dx.doi.org/10.1016/j.matchemphys.2014.05.0220254-0584/© 2014 Published by Elsevier B.V.

Please cite this article in press as: A. Mezni, eand Physics (2014), http://dx.doi.org/10.1016

g r a p h i c a l a b s t r a c t

� Hybrid AueZnO nanoparticles weresynthesized by a novel one-pot syn-thesis method that makes use of 1,3-propanediol.

� The polyol solvent 1,3-propanediolplays the roles of the reducing agentand the stabilizer layer.

� The AueZnO nanoparticles exhibit astrong localized surface plasmonresonance.

a r t i c l e i n f o

Article history:Received 2 September 2013Received in revised form29 March 2014Accepted 10 May 2014

Keywords:Chemical synthesisComposite materialsNanostructuresRaman spectroscopy and scatteringOptical properties

a b s t r a c t

In this work, we report on the synthesis of hybrid AueZnO nanoparticles using a one-pot chemicalmethod that makes use of 1,3-propanediol as a solvent, a reducing agent and a stabilizing layer. Theproduced nanoparticles consisted of Au cores decorated with ZnO nanoparticles. The structure andmorphology of the nanoparticles were characterized by transmission electron microscopy (TEM), X-raydiffraction (XRD), energy dispersive X-ray spectrometry (EDX) and Raman spectroscopy. Opticalextinction measurements, combined with numerical simulations, showed that the AueZnO nano-particles exhibit a localized surface plasmon resonance (SPR) clearly red-shifted with respect to that ofbare Au nanoparticles (AuNPs). This work contributes to the emergence of multi-functional nano-materials with possible applications in surface plasmon resonance based biosensors, energy-conversiondevices, and in water-splitting hydrogen production.

© 2014 Published by Elsevier B.V.

1. Introduction

Hybrid metalesemiconductor nanoparticles have attractedgreat attention from both, the fundamental basic scientific andtechnological points of view [1e4]. These nanocomposite materialsnot only combine the unique properties of the metal and thesemiconductor, but can also generate new properties due to themetalesemiconductor interface in coreeshell and Janus

t al., Synthesis of hybrid AueZ/j.matchemphys.2014.05.022

nanoparticles for instance. Indeed, the presence of such an interfacecan enhance the light absorption in the semiconductor and pro-mote effective charge separation which is required for efficientphotocatalytic applications [5e8]. AueZnO nanoparticles arenontoxic, biocompatible and chemically stable, and can thus beused in diverse areas such as multi-modal biological detection [9],catalysis [10], solar energy conversion [11] and opto-electronicsapplications [12].

Several chemistry-based methods have been proposed to syn-thesize hybrid metalesemiconductor nanoparticles [13e28]. Themain difficulty in preparing such particles lies in the weak inter-action between the semiconductor (e.g., ZnO, CdSe and TiO2) and

nO nanoparticles using a one pot polyol process, Materials Chemistry

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A. Mezni et al. / Materials Chemistry and Physics xxx (2014) 1e82

the metal (e.g., Au, Ag, Pt, and Pd). The key to form AueZnO hybridnanomaterials is to promote the heterogeneous growth of ZnO (orAuNPs) on Au (or ZnO) seeds. Recently, Li et al. [15] successfullyprepared AueZnO hybrid nanoparticles with hexagonal pyramid-like structure. The controlled synthesis of AueZnO hybrid NPswas based on the heterogeneous nucleation and the selectivegrowth of ZnO on pre-synthesized Au seeds dispersed in hexane.Lee et al. [18] synthesized AueZnO nanoparticles through thenucleation and decomposition of zinc hydroxide on the surface ofNaBH4-reduced AuNPs in ethanol. Xin Wang et al. [25] used ZnOnanocrystals as the seeding material for the nucleation and growthof citrate-reduced gold to form water-soluble dumbbell-shapedZnOeAuNPs.

Another strategy for the synthesis of AueZnO nanoparticlesconsists in using specific ligands as linkers with the affinity of theirfunctional groups to AuNPs and ZnO surfaces. Xianghong Liu et al.[26] reported a facile method for the assembly of noble metal (Auand Pt) nanoparticles onto ZnO rods using a green non-toxic re-agent amino acid lysine, with two amino functional groups as thecapping agent. Exploiting the affinity of thiol functional groups toAuNPs and ZnO surfaces, Whitten et al. [27] reported a simplestrategy to synthesize AueZnO nanoparticles by using dithiol as thelinker ligand.

So, in most cases, the synthesis of stable colloids of AueZnOnanoparticles requires the use of stabilizers or capping agents,several reagents and the reaction is generally carried out in severalsteps. In this work, we report the synthesis of ZnO-decoratedAuNPs formed in one-pot in 1,3-propanediol by using only gold(III) and zinc (II) precursors without the addition of any other re-agents, template or complex metal ligand. The polyol solvent playsthe role of both a complexant and a surfactant agent which adsorbson the nanoparticles' surface, thus preventing their agglomeration.

2. Experimental procedure

2.1. Synthesis of ZnO-decorated AuNPs

The synthesis of the ZnO-decorated AuNPs was achieved in aone-pot chemical process where gold salt HAuCl4 and zinc (II) ac-etate were mixed together in 1,3-propanediol (C3H8O2). Thesequential reactions were thermally controlled.

Au nanoparticles were initially formed by thermal reduction ofthe Au precursor at a moderate temperature. The thermal decom-position of zinc acetate dehydrate (Zn(OAc)2$2H2O) onto the sur-face of the preformed Au nanoparticles occurred at a hightemperature. The synthesis was carried out in a 100 ml three-neck

Fig. 1. XRD patterns of pure ZnO N

Please cite this article in press as: A. Mezni, et al., Synthesis of hybrid AueZand Physics (2014), http://dx.doi.org/10.1016/j.matchemphys.2014.05.022

flask equipped with a condenser, a mechanical stirrer and a ther-mograph. 0.038 mmol of HAuCl4$3H2O (purchased from Aldrich)were mixed with 0.17 mmol of zinc acetate dehydrate[(Zn(OAc)2$2H2O), Aldrich, AR grade] in 50 ml of 1,3-propanediol(ACROS Organics, 98%) with vigorous stirring. First, the mixturewas slowly heated to 150 �C and kept at that temperature for10min, then heated to 160 �C and kept at this temperature for 1 h. Aviolet homogeneous colloidal suspension was obtained. Aftercooling down to room temperature, the product was separated bycentrifugation, washed several times with ethanol/acetone (2:1)and re-dispersed in ethanol. After the centrifugation, the super-natant solution became clear and colorless, indicating that noAuNPs were present in the solution.

2.2. Structural and morphological characterization

The crystallographic structure of the so-obtained powder wascharacterized by X-ray diffraction (XRD) (using an INEL diffrac-tometer equipped with a cobalt anticathode (l ¼ 1.7890Å). Thecrystallite sizes were calculated using Scherrer's relation L ¼ 0.94l/bcos q, where l is the wavelength of the X-ray radiation, q and b are,respectively, the Bragg angle and full-width at half-maximum(FWHM) of the diffraction peak. The morphology of the particleswas determined by transmission electron microscopy (TEM) per-formed using a JEOL-JFC 1600 microscope operating at 100 keVaccelerating voltage. The chemical composition of the ZnO-decorated AuNPs was determined by energy-dispersive X-rayspectroscopy (EDX) attached to the TEM. High-resolution TEM(HRTEM) (Philips Tecnai F-20 SACTEM operating at 200 kV) imagesprovided further insight into the structure of the AueZnO NPs.

2.3. Optical characterization

The optical absorption spectra were acquired using a Per-kineElmer Lambda 11 UV/VIS spectrophotometer. The Raman ex-periments were carried out using a HoribaeJobineYvon XYspectrometer. We used the 363 nm Argon laser line to excite theRaman spectra close to the band gap of ZnO. The laser beam wasfocused onto the sample using a 50X objective. The laser intensitywas kept as low as possible in order to avoid sample heating anddegradation.

2.4. DDA simulations

Simulations of the optical extinction spectra were performedusing the discrete dipole approximation (DDA) implemented in

Ps and ZnO-decorated AuNPs.


Fig. 2. Raman scattering spectra of pure ZnO NPs and ZnO-decorated AuNPs excited at363 nm.

A. Mezni et al. / Materials Chemistry and Physics xxx (2014) 1e8 3

DDSCAT 7.2.2 software [29,30]. The wavelength-dependentrefractive indices of gold and bulk zinc oxide were taken fromJohnson and Christy [31] and from Hisashi et al. [32], respectively.

3. Results and discussion

3.1. Structural characterization

The crystalline phase of the nanoparticles was determined byXRD. Fig. 1 shows the XRD patterns of pure ZnO NPs and ZnO-decorated AuNPs. All the diffraction peaks of ZnO can be indexedto hexagonal wurtzite ZnO with the strong (100), (002), (101)

Fig. 3. TEM images (a, b) of the ZnO-decorated AuNPs. The hi


characteristic peaks (JCPDS No. 36-1451). The XRD pattern of theZnO-decorated AuNPs is very similar to that of pure ZnO NPs, thusindicating that the formation of Au in the reaction process has noinfluence on the crystal structure of the ZnO. Besides the diffractionpeaks of ZnONPs, three additional diffraction peaks were present at2q¼ 38.33, 44.21 and 64.79� and were assigned, respectively, to thediffraction lines of the (111), (200) and (220) planes of FCC gold(JCPDS No. 65-2870) [25]. The XRD results indicated that the syn-thesized nanoparticles have good crystallinity. The average size ofthe crystallites, estimated from the FWHM of the (100) diffractionpeak using Scherrer's relation, was of the order of 3.5 nm for theZnO NPs.

Further evidence for the formation of wurtzite ZnO around theAu cores was provided by the Raman scattering spectra shown inFig. 2. In wurtzite ZnO, phonons with A1, E1 and E2 symmetries areRaman active. Under resonant excitation, first and second orderresonant Raman scattering by E1(LO) phonons is dominant [33,34]as seen in Fig. 2. These Raman peaks are clearly visible thusattesting the good crystal quality of the ZnO nanoparticles sur-rounding the Au cores [35]. However, their linewidths are larger(nearly by a factor of 2) than those observed in pure ZnO nano-particles. Moreover, the Raman peaks of the AueZnO nanoparticlesare shifted towards lower wavenumbers as compared to pure ZnOnanoparticles; this is more pronounced for the 2E1(LO) secondharmonic peak. The fact that the Raman peaks are broader andshifted in the case of AueZnO nanoparticles can be attributed to theAueZnO interface. Indeed, it is well known that impurities, struc-tural defects and interfaces may lead to phonon localization thatresults in the Raman peak broadening and shift, and which aredirectly connected with the phonon dispersion curve [36]. In thecase of E1(LO) phonons, the vibrational frequency decreases withincreasing wavevector [37]. Hence, a down shift and a broadeningof the Raman line are expected in the case of E1(LO) phonons. It isinteresting to notice that the Raman scattering is enhanced in the

stogram in (c) shows the size distribution of the Au core.


Fig. 4. EDX spectrum of the ZnO-decorated AuNPs.


AueZnO NPs relative to pure ZnO NPs. Wang et al. [25] alsoobserved the enhancement of the Raman scattering in bifunctionalZnOeAu nanocomposites. The reason may be the electric field atthe AueZnO interface which increases the electronephononinteraction and hence the Raman intensity [38].

As shown by the transmission electronmicroscopy, presented inFig. 3, the nanoparticles consist mainly of faceted quasi-sphericalgold cores (around 10e40 nm) surrounded by closely packed zincoxide NPs (3e5 nm) forming a decoration. The size distribution ofthe Au core is shown in Fig. 3c. The average size of the Au core isaround 23.2 nm.

The EDX spectrum presented in Fig. 4, indicates that the nano-particles are of a high purity, since only Au, O and Zn elements aredetected. The presence of Cu is due to the copper grid used for the

Fig. 5. Low resolution TEM image (a) and H


TEM/EDX experiments, the Fe and Co elements are due to the polecomponents of the microscope.

The high-resolution TEM (HRTEM) images of the ZnO-decoratedAuNPs are shown in Fig. 5. A strong interface contiguity between theAu and the ZnO nanoparticles is observed. From the HRTEM image(Fig. 5c, d), the interplanar spacing of the ZnO (002) atomic plane is0.26 nm, in agreement with the wurtzite ZnO structure [25]. On theother hand, it is evident from the HRTEM images that the AuNPsexhibit “moir�e” fringes which suggest that the Au and ZnO latticesare gradually displaced from each other or rotated. This indicatesthat the Au/ZnO interface is not coherent, which is often the case inlattice-mismatched metal-oxide systems [39]. As a matter of fact,the epitaxial nucleation and growth of ZnO on the surface of Auwasnot observed in this study. The reason why hybrid AueZnO NPs do

RTEM of ZnO-decorated AuNPs (bed).


https://www.researchgate.net/publication/230823217_Transmission_Electron_Microscopy_A_Textbook_for_Materials_Science_III._Imaging?el=1_x_8&enrichId=rgreq-e486d40b-cb3b-48cb-807d-358b660de033&enrichSource=Y292ZXJQYWdlOzI2NDQ5ODQ0NztBUzoxNDc3OTE3OTU5ODY0MzJAMTQxMjI0NzcxODc0Mw==

Fig. 6. Schematic of the formation mechanism of the ZnO-decorated AuNPs in 1,3-propanediol.

Fig. 7. (a) TEM images of AueZnO NPs prepared with a higher zinc acetate concentration (�10), (b) selected area diffraction (SAED) patterns of AueZnO, (c) high-resolutiontransmission electron microscope (HRTEM) images and (d) typical EELS spectra from selected nanoparticles.


Please cite this article in press as: A. Mezni, et al., Synthesis of hybrid AueZnO nanoparticles using a one pot polyol process, Materials Chemistryand Physics (2014), http://dx.doi.org/10.1016/j.matchemphys.2014.05.022

Fig. 8. Secondary electrons STEM image and EDX maps at the Zn, O and Au signals. The lower panel shows the EDX profile of the Zn (green), O (blue) and Au (red) across the lineshown in top right panel. (For interpretation of the references to color in this figure legend, the reader is referred to the web version of this article.)


not form a core/shell structure is the difference between theircrystalline structures, i.e., Au is cubic and ZnO is hexagonal [18].

3.2. Formation mechanism

The observations showed that the solution color changed fromyellow to purple at 100 �C. This coloration was visible until thetemperature reached 150 �C. Above this temperature, and up to160�, the solution became milky with some turbidity. These ob-servations suggest a sequential formation process.

First, the change of color from yellow to purple observed at100 �C reveals the formation of Au nanoparticles. Indeed, based onour previous study [40] and many other reports [41,42], the for-mation of AuNPs in a polyol medium is accompanied by a change inthe colloidal solution color (e.g. from yellow to pale in 1,2


propanediol reflecting the formation of gold nanoplates [41], fromyellow to blue in triethylene glycol [40], from light yellow topinkish violet in glycerol [42]). The stability of these nanoparticlesis ensured by the polyol molecules (1,3-propanediol in our case)grafted to the Au surface via electrostatic bonds [40].

With increasing temperature, the zinc acetate starts to decom-pose at the reactive Au surface to form an intermediate zinc hy-droxide [43]. Indeed, at 150 �C the solution becomes milky withsome turbidity, this could be attributed to the spontaneous for-mation of zinc hydroxide arising from the reaction of 1,3-propanediol with the zinc acetate [43]. The zinc hydroxide at theAu surface acts as a nucleation site for the growth of zinc oxide viainorganic polymerization reactions [44] thus leading to ZnO nuclei[43]. At 160 �C, further nucleation and growth of the ZnO takesplace. Because heterogeneous nucleation is preferred over



homogeneous nucleation [45], Zn ions tend to condense on pre-existing zinc oxide seeds already present at the surface of theAuNPs, rather than forming new nuclei in the solution. We believethat the 1,3-propanediol solvent plays a crucial role in the forma-tion of ZnO-decorated AuNPs. As a matter of fact, when the syn-thesis was conducted in ethylene glycol (EG) or diethylene glycol(DEG) using the same precursors, individual ZnO NPs and AuNPswere formed instead of hybrid AueZnO NPs.

We suggest that the formation of the hybrid AueZnO NPs isbased on an initial production of the Au nanoparticles followed by ahydroxylationecondensation process of an intermediate zinc hy-droxide, onto the surface of the preformed Au nanoparticles. Theproposed chemical reaction mechanism is described in Fig. 6. It canbe divided into 4 steps: formation of AuNPs in the polyol solvent(a), decomposition of the Zn (II) precursor at the surface of thepreformed AuNPs and formation of an intermediate zinc hydroxide(b), nucleation of ZnO seeds (c) and growth of the ZnO at the AuNPssurface leading to hybrid AueZnO NPs (d).

When the reaction was carried out under the same experi-mental conditions but with the zinc acetate concentrationincreased by a factor 10, nanoparticles around 140 nm in size andwith strong surface roughness are observed. The selected areaelectron diffraction (SAED) ring patterns clearly show the FCC Auand wurtzite ZnO phases (Fig. 7b). The High-Resolution TEM(HRTEM) image in Fig. 7c shows well-defined ZnO crystal planesthus corroborating the crystalline structure of the formed particles.The EELS spectra show (Fig. 7d) loss peaks corresponding to zinc(Zn L23) and oxygen (O K) only.

In order to investigate more precisely the composition of thesenanoparticles, we have performed a mapping of the EDX signal(Fig. 8). As can be seen, the nanoparticles consist mainly in ZnO. TheAu atomic percentage does not exceed 1e2% as evidenced by theconcentration profile in Fig. 8. It may reach 5% at some particularlocations of the nanoparticle but in general the Au concentration issmall. This shows that the control of the zinc acetate versus Auprecursor concentration is critical since increasing the zinc acetateconcentration does not result in a coreeshell AueZnO nano-particles with a larger ZnO coverage.

Fig. 9. Measured and calculated Extinction spectra of bare Au nanoparticles and ZnO-decorated AuNPs dispersed in ethanol. The surface plasmon bands, in the measuredspectra (continuous line) of the bare Au nanoparticles and ZnO-decorated AuNPs arepeaking at 533 and 568 nm, respectively. The extinction spectra of bare Au nano-particles and ZnOeAu coreeshell nanoparticles simulated using DDA are plotted asdashed lines. In the simulations, the diameter of the spherical Au core is 25 nm and theZnO shell thickness is 10 nm.


3.3. Optical properties

Themeasured optical extinction spectrum of the ZnO-decoratedAuNPs (corresponding to Figs. 3 and 5) is shown in Fig. 9. Thespectrum of 25 nm spherical bare gold NPs is also shown forcomparison. The extinction spectrum of the ZnO-decorated AuNPsclearly shows a surface plasmon resonance peaking at around568 nm, red-shifted by 35 nm with respect to the surface plasmonresonance of the bare AuNPs. This red-shift is due to the increase inthe optical index of the medium surrounding the gold cores [46].Indeed, the optical index of (bulk) ZnO is around 2.1 (orientationaveraged) which is much larger than that of ethanol (1.36). Thisred-shift is confirmed by the DDA simulations performed for 25 nmspherical AuNPs surrounded by a 10 nm spherical ZnO shell. Thespectra calculated for the bare AuNPs and for the AueZnO coree-shell NPs are in satisfactory agreement with the measured ones.However, the experimental linewidth of the surface plasmonresonance is clearly larger than the simulated one probably becauseof inhomogeneous broadening due to size and shape fluctuations ofthe nanoparticles.

4. Conclusion

Summing up, we have reported the synthesis of hybrid AueZnOnanoparticles with a controlled morphology and high crystallinequality using a one pot polyol process, without adding any otherreagents, template or complex metal ligand. The 1,3-propanediolsolvent plays the role of both a reducing agent and a stabilizinglayer.

The formation mechanism of ZnO NPs in 1,3-propanediol facil-itates and guides the reaction to the formation of the ZnO-decorated AuNPs. The temperature control of the spontaneousnucleation step followed by a well-separated growth step, explainthe homogeneity in size and morphology of the obtained hybridnanoparticles.

Because of the simplicity of the process, we believe that thisstrategy is suitable for the scalable production of hybrid nano-composite materials. On the other hand, because of their uniquestructure, the ZnO-decorated AuNPs are expected to provide newinsights into various application fields including plasmonicenhanced photocatalysis, hydrogen production via solar-lightinduced water splitting and for chemical and biological sensing,as well as for medical applications [47,48].

Acknowledgments

Amine Mezni, gratefully acknowledges the support of the Min-istry of Higher Education and Scientific Research of Tunisia. Thiswork has also been supported by the CALMIP high-performancecomputing facilities center at the Paul Sabatier University of Tou-louse. The authors are also grateful to S�ebastien Jouli�e for the EDXmapping measurements.

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