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Ag Nanoparticles prepared by laser ablation in liquid
Materials Science in Semiconductor Processing 105 (2020) 104712
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Materials Science in Semiconductor Processing journal homepage: www.elsevier.com/locate/mssp
Optical and structural investigation of synthesis ZnO/Ag Nanoparticles prepared by laser ablation in liquid
T
Rahma Anugrahwidyaa, Nurfina Yudasarib, Dahlang Tahira,∗ a b
Department of Physics, Hasanuddin University, Makassar, 90245, Indonesia Research Center for Physics, Indonesia Institute of Sciences, PUSPIPTEK, Tangerang Selatan, 15314, Indonesia
A R T I C LE I N FO
A B S T R A C T
Keywords: ZnO/Ag nanoparticles Laser ablation Photoluminescence Band gap TEM
ZnO/Ag nanoparticle was synthesis by using pulsed laser ablation in liquid with various Ag doped at a time of 1, 3, and 5 min. Characterization was carried out with UV–Vis (UV–Visible) Spectrometer, PL 325 (Photoluminescence 325) spectrometer, XRD (X-Ray diffraction), and TEM (transmission electron microscopy). The enhancement of dopant time, the band gap value decrease from 3,021 eV to 2,781 eV and the wavelength peak position was shifted to the red shift which can transform the structure of ZnO nanoparticles and can be applied as food packaging in the future.
1. Introduction Zinc oxide (ZnO) is described as a functional, strategic, promising, and versatile inorganic material with a broad range of applications [1–4]. It has been studied for its optical, structure properties, photocatalytic, and many other important characteristic [5–9]. It also becomes particular interest because it is not only stable under harsh process conditions, but also generally regarded as safe materials to human beings [10,11]. Further, some essential ZnO nanostructures parameter, including particle size and concentration, morphology, surface charges, surface defects, and UV-Illumination have been modified and studied. In particular, the inclusion of silver (Ag) in the synthesis of ZnO nanostructures has gained number of attention [12,13]. Furthermore, as a dopant, Ag has a lot of potential to produce defects aiming to increase the catalytic activity in ZnO nanostructures [14,15]. Nevertheless, the chemical methods are still dominating the synthesis methods of ZnO/Ag nanostructures [16–19]. Chemical methods have some issues regarding metal precursor, reductant, stabilizing and capping agents which are always required to produce and ensure stable chemical-synthesized colloids, which can be toxic for the living creatures [20,21]. Laser ablation in liquid (LAL) technique allows metals and metal oxides nanoparticles synthesis without metal precursors and reductant or capping agents [22–24]. The produced nanoparticles were relatively higher purity in comparison to those prepared with chemical methods. Some of work has been done on applying LAL technique to produce
∗
nanoparticles with two different metal/metal oxide elements [25–28]. Zhao et al. has reported the synthesis of core/shell structured of Ag/ ZnO, and elaborated its optical and structure properties. Khasnan et al. also has claimed for successfully applying LAL technique for Mg doped ZnO nanostructures. However, to the best of our knowledge, optical and structural characteristic of Ag doped ZnO nanoparticle by using LAL technique has not been reported. Hence, we present our work regarding the synthesis of ZnO doped Ag nanoparticles including optical and structural behavior of our ZnO/Ag nanoparticles synthesized by LAL. 2. Experimental The ZnO/Ag nanoparticles were synthesis by two-step method. As can be seen the experimental setup in Fig. 1. First, a 3 mm thick zinc plate was placed on the bottom of a rotating platform at 5 rpm in 5 ml aquabides. The laser Nd:YAG was set up at the wavelength 1064 nm, 100 mJ energy laser, and pulsed duration 160 μs was focused on the zinc plate to (1.6 × 1.6 cm). The Zinc plate was ablated for 30 min. Second, a silver plate was ablated by the same pulsed energy of laser in the ZnO colloid synthesis similar with the first step for 1, 3, and 5 min for producing the ZnO/Ag nanoparticles. The silver nanoparticles were synthesis by the same energy laser by ablation of a silver plate in 5 ml aquabides for 5 min. An UV–Visible spectrophotometer, a photoluminescence 325 spectrometer, the x-ray diffraction spectrum (XRD) and transmission electron microscopy (TEM) were used to identify optical properties, structure and morphology of the ZnO/Ag nanoparticles produced by ablation process.
Corresponding author. E-mail address: [email protected] (D. Tahir).
https://doi.org/10.1016/j.mssp.2019.104712 Received 6 July 2019; Received in revised form 31 August 2019; Accepted 2 September 2019 1369-8001/ © 2019 Published by Elsevier Ltd.
Materials Science in Semiconductor Processing 105 (2020) 104712
R. Anugrahwidya, et al.
characterized by using UV–Vis absorption and PL spectroscopies. The UV–Vis absorption spectra ZnO/Ag nanoparticles were shown in Fig. 3. The spectrum of pure ZnO nanoparticles shows a broad spectrum from 300 to 400 nm. Pure ZnO nanoparticles show UV absorption edge at 335 nm and for pure Ag nanoparticles at 407 nm. Silver which adding to ZnO nanoparticles shifted from the absorption edge toward to the major wavelength (red shift) due to the bye Zn metal was ablated by using laser. The resulting nanoparticles will come out and spread into the liquid (aquabides) and bonding with oxygen. When Ag atoms doped into ZnO, Ag atoms will transform position of Zn in the ZnO lattice [29]. Transformation of the absorption after the addition of the dopant, shows transformation in band structure and decrease in the band gap of ZnO without doping. The optical energy gap of the nanoparticles was formulated by Ref. [30]:
Fig. 1. Synthesis method of the ZnO/Ag nanoparticles.
Eg
3. Result and discussion The ZnO/Ag nanoparticles were synthesis by pulsed laser ablation. This synthesis is aim to the characterization of ZnO/Ag nanoparticles and physical properties colloid color from ZnO/Ag in Fig. 2. Color of ZnO colloid nanoparticles was grayish white. By doping Ag metal, the color of colloid was turns brownish yellow, it's caused by colloid of Ag which synthesis by using laser ablation will produce a yellow gold color. Nanoparticle were ablated on the surface of metal plate, create colloid discoloration as confirmed by Table 1. Table 1 shows that mass of Zn metal plate has decreased after ablation for 30 min. The average difference is 0.0011 g. The effect of 0.0011 g nanoparticles in 5 ml ZnO/Ag colloid will affect to the amount of the atomic in solution. Mass of Ag plates also decreased after ablation for 5 min and the mass of ZnO doped by Ag also has decrease. This shows, every additional time of ablation, more nanoparticles were released from the surface of the metal plate contribute to the amount of atoms in solution. The longer of the surface of the metal plate is ablated resulting more nanoparticles are spread into the liquid. It causes the mass of the plate will decrease in each additional time ablation. This is creating the discoloration of were nanoparticle colloid. The optical properties of the pure and ZnO doped Ag sample were
Table 1 Measurement of metal plate mass.
1 2 3 4 5 6
Zinc Plate
Silver Plate
Ablation Time
Before (gram)
After (gram)
Ablation Time
Before (gram)
After (gram)
30 min
5.9808 5.9675 5.9604 5.9553 5.9460 5.9378
5.9798 5.9660 5.9594 5.9545 5.9449 5.9368
1 min 2 min 3 min 4 min 5 min 5 min
3.5696 3.5679 3.5663 3.5624 3.5585 3.5554
3.5695 3.5677 3.5660 3.5620 3.5580 3.5549
and ??? = (2.303 × A × hυ)n
(1)
where, A is absorption, һ is Planck's constant, υ is light frequency, λ is wavelength, һυ is foton energy (eV), n = 1 and Eg is energy gap. ZnO band gap is 3.021 eV, ZnO/Ag for 1 min ablated is 2.864 eV, ZnO/Ag for 3 min is 2.851 eV, and ZnO/Ag for 5 min is 2.781 eV. Decreasing energy gap along increasing concentration (time the ablation) can affect the quality of colloid nanoparticles. The increasing concentration of dopants causes the colloids become yellow because Ag molecules involved thus by affect the agglomeration process. Energy gap indicates the movement of electrons across from valence band towards conduction band. The smaller band gap value indicates that more electrons across in the excitation area which can affected to the absorbance intensity of the nanoparticles. The absorbance intensity shows the transition activity from the excitation area to the ground state. The results of this research obtained intensity increase along ablation time increased. The larger absorbance intensity was measured, more electron across in the excitation area and the large emissions were produced. Further information about the optical properties of ZnO can be seen from PL spectra. The PL emission spectrum of the synthesis of ZnO and ZnO/Ag nanoparticles is shown in Fig. 4. The first emission spectrum of ZnO nanoparticles is at wavelength of 396.5 nm with energy gap is 3.13 eV and the second spectrum peak is in green shift at wavelength of 548.3 nm (2.26 eV). This clearly shows a shift in emission peaks from higher to lower regions of photon energy. The emission peak at 396.5 nm indicates the presence of ZnO arising due to the recombination of holes and electrons in the valence band and in the conduction band. A shift towards green shift (548.3 nm) is caused by the electron displacement from Fermi level to conduction band ZnO material, which the leads to the band gap widening and identify as a defects and impurities in ZnO nanoparticles [31]. The first emission spectrum of ZnO doping Ag 1 min, 3 min and 5 min respectively is in the blue shift area at wavelength of 400.4 nm, 411.6 nm and 422.3 nm. These results indicate a significant shifting at transmittance of 360–450 nm wavelength range, which is the range of the ultraviolet or blue shift wavelength region. The enhancement of transmittance values indicates that colloid are homogeneous which is in this case there is an electron displacement from the base to the excited state. This is also similar to previous studies, which indicates a wavelength shift in the near band edge (NBE) area to deep level emissions (DLE) after the addition of Ag dopants. These phenomena are caused by recombination of electrons and holes in conduction band. Where, Ag is a donor and facilitate the transformation the structure of ZnO indicated by wavelength widening [31–33]. The second emission spectrum of ZnO/Ag 1 min respectively and ZnO/Ag 3 min are in the green shift area at wavelength of 565 nm and 572 nm, the shifted to the green shift is caused by the electron displacement from Fermi level to the conduction band of ZnO material and also due to the donor or dopant which leads to the band gap widening [31]. Addition of Ag concentration (long of ablation time) decreases
Fig. 2. Colloid ZnO/Ag nanoparticle (a) ZnO Colloid (b) ZnO/Ag 1 min (c) ZnO/Ag 2 min (d) ZnO/Ag 3 min (e) ZnO/Ag 4 min (f) ZnO/Ag 5 min (g) Ag Colloid.
No
hυ λ
2
Materials Science in Semiconductor Processing 105 (2020) 104712
R. Anugrahwidya, et al.
Fig. 3. UV–Vis absorption spectra of pure ZnO, ZnO doped Ag and Ag (a) Band gap of ZnO/Ag nanoparticles (b).
intensity in green shift region. This is due to the presence of intrinsic defects, such as oxygen vacancy. However, in ZnO/Ag 5 min, a peak is formed in green shift region but the peak is not the same as the other peaks due to the concentration of Ag was different. It was concluded that the enhanced of the concentration of dopant Ag could affect the result of the emission and intensity. According to Zhang, emission of Ag peak at wavelength of 330 nm. Furthermore, Ag concentration addition into ZnO, ZnO/Ag will be red shift [34]. XRD spectrum was used to determine the crystal structure of colloid nanoparticles. XRD analysis of ZnO, ZnO/Ag and Ag nanoparticles is shown in Fig. 5. The result of ZnO nanoparticles shows all the peaks had a hexagonal wurtzite crystal structure, it because the structure of the results was almost the same as the previous study [31]. No other phase was observed which shows no inclusion of Zn in ZnO, which corresponds to the UV–Vis spectrum [35,36]. Based on the XRD results, ZnO peaks were detected at 31.79°, 34,52°, 36,24°, 47.73°, 56.56° and 62.81° with hkl values respectively (101), (002), (100), (102), (110), and (103). Ag peak is formed at 38.11°, 44.36°, 66.47° and 77.39° with hkl values in a row (111), (200), (220), and (311). The results were calculated by using Scherrer equation [31]:
Fig. 4. PL Spectra of Pure ZnO and Ag doped ZnO nanoparticles.
Fig. 5. XRD patterns of ZnO/Ag Nanoparticles. 3
Materials Science in Semiconductor Processing 105 (2020) 104712
R. Anugrahwidya, et al.
Fig. 6. TEM image and Particle Size Distribution of Pure ZnO (a) Pure Ag (b) ZnO/Ag 1 min (c) ZnO/Ag 3 min (d) ZnO/Ag 5 min (e).
4
Materials Science in Semiconductor Processing 105 (2020) 104712
R. Anugrahwidya, et al.
D=
0.9 λ β Cos θ
particle size is about 21 nm clearly. Acknowledgements
where D is the average crystal size (nm), λ = 1.54056 Å is the wavelength of the radiation., β is the width at half maximum intensity in radians at 2θ (°) and θ is Diffraction angle (Bragg Angle). Doping is a way to change the electrical and optical properties of semiconductors. One of the purposes of doping is to enhancement the conductivity of ZnO. Ag is an element that can be used as a dopant because it can be an absorber to collect photoelectrons that produced from ZnO conduction bands, it can be effective for inhibit electron-hole recombination [30]. Based on the XRD analysis results, the diffraction peaks were obtained on each ZnO nanoparticles which doped by Ag with doping time variations of 1 min, 3 min and 5 min. At ZnO/Ag 1 min peaks are formed at angle of 2θ: 28.13°, 31.78°, 34.43°, 36.22°, 47.65° with an average crystal size is 11.0577 nm. At ZnO/Ag 3 min, peaks are formed at angle of 2θ: 29.0°, 31.73°, 34.36°, 36,19°, 47.62° with an average crystal size is 14.7711 nm for ZnO/Ag 5 min, peaks are formed at angle of 2θ: 28.91°, 31.73°, 34.43°, 36.2°, 47.44° with an average crystal size is 10.6467 nm. From the results, peak Ag on ZnO doped at 2θ = 38.11° is invisible as shown in Fig. 5. It's because Ag+ ions behave as monovalent dopants, which have the ability to cover both lattices and interstitial sites because of high radius ion Ag+. The effect of combining Ag in the ZnO lattice was studied by monetizing the position and binding of the diffraction peak which is influenced by the level of operation due to the incorporation of Ag [32]. However, observed at angle of 2θ: 35°–37°, the peak shift occurs at angle of 36.0°–36.3°. Each enhancement of dopant concentration, the peak formed will lead to the left. It's indicates that Ag managed to be a dopant and not core/shell, the enhancement of Ag doesn't change the phase or lattice of ZnO nanoparticles and any enhancement of Ag to ZnO concentration also increases the intensity. Morphological analysis of ZnO, ZnO/Ag and Ag nanoparticles was tested by using TEM. The results show the morphological form of ZnO without Ag doping and after Ag dopant was shown in Fig. 6. The results show, the form of ZnO nanoparticles with a magnification of 50 nm are nanorods whereas the shape of Ag nanoparticles with the same magnification is sphere, which are shown in Fig. 6 (a) and (b). The color of Ag nanoparticles is dark predominantly than ZnO, it's because Ag has a large atomic number and the nanoparticles synthesis results shows, Ag colloid is more concentrated than ZnO colloid which tends to be grayish. After the enhancement of Ag dopant, transforms the structure, from nanorod structure to the sphere structure along with the enhancement of concentration as an effect of Ag doping in Fig. 6 (c), (d), and (e). It shows, if Ag is aggregate and there are several agglomeration points as the effect of Ag. In addition, agglomeration causes color differences. The darker color, indicates that more crystal is accumulated at each other at a certain point. Based on the TEM data analysis, the average ZnO and Ag nanoparticles is around 13–20 nm and 10–35 nm (see Fig. 6) which is due to be XRD analysis. Also, the average for ZnO doping Ag with 1, 3 and 5 min ablation is around 10–20 nm.
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4. Conclusion ZnO/Ag nanoparticle had been successfully synthesized by using pulsed laser ablation in liquid with various Ag doped at a time of 1, 3, and 5 min. The structural, optical, particle size, and anti-bacterial properties of ZnO/Ag nanoparticles were investigated. Based on the result, the enhancement of dopant time, the band gap value will decrease, so peak wavelength shift to the red shift was confirmed by photoluminescence 325 spectrometer. The average particle size of ZnO/ Ag nanoparticles on analysis XRD spectra is 12.1585 nm. TEM image for ZnO nanoparticles is nanorods, Ag nanoparticles is round and ZnO/Ag nanoparticles showed combination of nanorods and nanosphere with 5
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Contents lists available at ScienceDirect
Materials Science in Semiconductor Processing journal homepage: www.elsevier.com/locate/mssp
Optical and structural investigation of synthesis ZnO/Ag Nanoparticles prepared by laser ablation in liquid
T
Rahma Anugrahwidyaa, Nurfina Yudasarib, Dahlang Tahira,∗ a b
Department of Physics, Hasanuddin University, Makassar, 90245, Indonesia Research Center for Physics, Indonesia Institute of Sciences, PUSPIPTEK, Tangerang Selatan, 15314, Indonesia
A R T I C LE I N FO
A B S T R A C T
Keywords: ZnO/Ag nanoparticles Laser ablation Photoluminescence Band gap TEM
ZnO/Ag nanoparticle was synthesis by using pulsed laser ablation in liquid with various Ag doped at a time of 1, 3, and 5 min. Characterization was carried out with UV–Vis (UV–Visible) Spectrometer, PL 325 (Photoluminescence 325) spectrometer, XRD (X-Ray diffraction), and TEM (transmission electron microscopy). The enhancement of dopant time, the band gap value decrease from 3,021 eV to 2,781 eV and the wavelength peak position was shifted to the red shift which can transform the structure of ZnO nanoparticles and can be applied as food packaging in the future.
1. Introduction Zinc oxide (ZnO) is described as a functional, strategic, promising, and versatile inorganic material with a broad range of applications [1–4]. It has been studied for its optical, structure properties, photocatalytic, and many other important characteristic [5–9]. It also becomes particular interest because it is not only stable under harsh process conditions, but also generally regarded as safe materials to human beings [10,11]. Further, some essential ZnO nanostructures parameter, including particle size and concentration, morphology, surface charges, surface defects, and UV-Illumination have been modified and studied. In particular, the inclusion of silver (Ag) in the synthesis of ZnO nanostructures has gained number of attention [12,13]. Furthermore, as a dopant, Ag has a lot of potential to produce defects aiming to increase the catalytic activity in ZnO nanostructures [14,15]. Nevertheless, the chemical methods are still dominating the synthesis methods of ZnO/Ag nanostructures [16–19]. Chemical methods have some issues regarding metal precursor, reductant, stabilizing and capping agents which are always required to produce and ensure stable chemical-synthesized colloids, which can be toxic for the living creatures [20,21]. Laser ablation in liquid (LAL) technique allows metals and metal oxides nanoparticles synthesis without metal precursors and reductant or capping agents [22–24]. The produced nanoparticles were relatively higher purity in comparison to those prepared with chemical methods. Some of work has been done on applying LAL technique to produce
∗
nanoparticles with two different metal/metal oxide elements [25–28]. Zhao et al. has reported the synthesis of core/shell structured of Ag/ ZnO, and elaborated its optical and structure properties. Khasnan et al. also has claimed for successfully applying LAL technique for Mg doped ZnO nanostructures. However, to the best of our knowledge, optical and structural characteristic of Ag doped ZnO nanoparticle by using LAL technique has not been reported. Hence, we present our work regarding the synthesis of ZnO doped Ag nanoparticles including optical and structural behavior of our ZnO/Ag nanoparticles synthesized by LAL. 2. Experimental The ZnO/Ag nanoparticles were synthesis by two-step method. As can be seen the experimental setup in Fig. 1. First, a 3 mm thick zinc plate was placed on the bottom of a rotating platform at 5 rpm in 5 ml aquabides. The laser Nd:YAG was set up at the wavelength 1064 nm, 100 mJ energy laser, and pulsed duration 160 μs was focused on the zinc plate to (1.6 × 1.6 cm). The Zinc plate was ablated for 30 min. Second, a silver plate was ablated by the same pulsed energy of laser in the ZnO colloid synthesis similar with the first step for 1, 3, and 5 min for producing the ZnO/Ag nanoparticles. The silver nanoparticles were synthesis by the same energy laser by ablation of a silver plate in 5 ml aquabides for 5 min. An UV–Visible spectrophotometer, a photoluminescence 325 spectrometer, the x-ray diffraction spectrum (XRD) and transmission electron microscopy (TEM) were used to identify optical properties, structure and morphology of the ZnO/Ag nanoparticles produced by ablation process.
Corresponding author. E-mail address: [email protected] (D. Tahir).
https://doi.org/10.1016/j.mssp.2019.104712 Received 6 July 2019; Received in revised form 31 August 2019; Accepted 2 September 2019 1369-8001/ © 2019 Published by Elsevier Ltd.
Materials Science in Semiconductor Processing 105 (2020) 104712
R. Anugrahwidya, et al.
characterized by using UV–Vis absorption and PL spectroscopies. The UV–Vis absorption spectra ZnO/Ag nanoparticles were shown in Fig. 3. The spectrum of pure ZnO nanoparticles shows a broad spectrum from 300 to 400 nm. Pure ZnO nanoparticles show UV absorption edge at 335 nm and for pure Ag nanoparticles at 407 nm. Silver which adding to ZnO nanoparticles shifted from the absorption edge toward to the major wavelength (red shift) due to the bye Zn metal was ablated by using laser. The resulting nanoparticles will come out and spread into the liquid (aquabides) and bonding with oxygen. When Ag atoms doped into ZnO, Ag atoms will transform position of Zn in the ZnO lattice [29]. Transformation of the absorption after the addition of the dopant, shows transformation in band structure and decrease in the band gap of ZnO without doping. The optical energy gap of the nanoparticles was formulated by Ref. [30]:
Fig. 1. Synthesis method of the ZnO/Ag nanoparticles.
Eg
3. Result and discussion The ZnO/Ag nanoparticles were synthesis by pulsed laser ablation. This synthesis is aim to the characterization of ZnO/Ag nanoparticles and physical properties colloid color from ZnO/Ag in Fig. 2. Color of ZnO colloid nanoparticles was grayish white. By doping Ag metal, the color of colloid was turns brownish yellow, it's caused by colloid of Ag which synthesis by using laser ablation will produce a yellow gold color. Nanoparticle were ablated on the surface of metal plate, create colloid discoloration as confirmed by Table 1. Table 1 shows that mass of Zn metal plate has decreased after ablation for 30 min. The average difference is 0.0011 g. The effect of 0.0011 g nanoparticles in 5 ml ZnO/Ag colloid will affect to the amount of the atomic in solution. Mass of Ag plates also decreased after ablation for 5 min and the mass of ZnO doped by Ag also has decrease. This shows, every additional time of ablation, more nanoparticles were released from the surface of the metal plate contribute to the amount of atoms in solution. The longer of the surface of the metal plate is ablated resulting more nanoparticles are spread into the liquid. It causes the mass of the plate will decrease in each additional time ablation. This is creating the discoloration of were nanoparticle colloid. The optical properties of the pure and ZnO doped Ag sample were
Table 1 Measurement of metal plate mass.
1 2 3 4 5 6
Zinc Plate
Silver Plate
Ablation Time
Before (gram)
After (gram)
Ablation Time
Before (gram)
After (gram)
30 min
5.9808 5.9675 5.9604 5.9553 5.9460 5.9378
5.9798 5.9660 5.9594 5.9545 5.9449 5.9368
1 min 2 min 3 min 4 min 5 min 5 min
3.5696 3.5679 3.5663 3.5624 3.5585 3.5554
3.5695 3.5677 3.5660 3.5620 3.5580 3.5549
and ??? = (2.303 × A × hυ)n
(1)
where, A is absorption, һ is Planck's constant, υ is light frequency, λ is wavelength, һυ is foton energy (eV), n = 1 and Eg is energy gap. ZnO band gap is 3.021 eV, ZnO/Ag for 1 min ablated is 2.864 eV, ZnO/Ag for 3 min is 2.851 eV, and ZnO/Ag for 5 min is 2.781 eV. Decreasing energy gap along increasing concentration (time the ablation) can affect the quality of colloid nanoparticles. The increasing concentration of dopants causes the colloids become yellow because Ag molecules involved thus by affect the agglomeration process. Energy gap indicates the movement of electrons across from valence band towards conduction band. The smaller band gap value indicates that more electrons across in the excitation area which can affected to the absorbance intensity of the nanoparticles. The absorbance intensity shows the transition activity from the excitation area to the ground state. The results of this research obtained intensity increase along ablation time increased. The larger absorbance intensity was measured, more electron across in the excitation area and the large emissions were produced. Further information about the optical properties of ZnO can be seen from PL spectra. The PL emission spectrum of the synthesis of ZnO and ZnO/Ag nanoparticles is shown in Fig. 4. The first emission spectrum of ZnO nanoparticles is at wavelength of 396.5 nm with energy gap is 3.13 eV and the second spectrum peak is in green shift at wavelength of 548.3 nm (2.26 eV). This clearly shows a shift in emission peaks from higher to lower regions of photon energy. The emission peak at 396.5 nm indicates the presence of ZnO arising due to the recombination of holes and electrons in the valence band and in the conduction band. A shift towards green shift (548.3 nm) is caused by the electron displacement from Fermi level to conduction band ZnO material, which the leads to the band gap widening and identify as a defects and impurities in ZnO nanoparticles [31]. The first emission spectrum of ZnO doping Ag 1 min, 3 min and 5 min respectively is in the blue shift area at wavelength of 400.4 nm, 411.6 nm and 422.3 nm. These results indicate a significant shifting at transmittance of 360–450 nm wavelength range, which is the range of the ultraviolet or blue shift wavelength region. The enhancement of transmittance values indicates that colloid are homogeneous which is in this case there is an electron displacement from the base to the excited state. This is also similar to previous studies, which indicates a wavelength shift in the near band edge (NBE) area to deep level emissions (DLE) after the addition of Ag dopants. These phenomena are caused by recombination of electrons and holes in conduction band. Where, Ag is a donor and facilitate the transformation the structure of ZnO indicated by wavelength widening [31–33]. The second emission spectrum of ZnO/Ag 1 min respectively and ZnO/Ag 3 min are in the green shift area at wavelength of 565 nm and 572 nm, the shifted to the green shift is caused by the electron displacement from Fermi level to the conduction band of ZnO material and also due to the donor or dopant which leads to the band gap widening [31]. Addition of Ag concentration (long of ablation time) decreases
Fig. 2. Colloid ZnO/Ag nanoparticle (a) ZnO Colloid (b) ZnO/Ag 1 min (c) ZnO/Ag 2 min (d) ZnO/Ag 3 min (e) ZnO/Ag 4 min (f) ZnO/Ag 5 min (g) Ag Colloid.
No
hυ λ
2
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Fig. 3. UV–Vis absorption spectra of pure ZnO, ZnO doped Ag and Ag (a) Band gap of ZnO/Ag nanoparticles (b).
intensity in green shift region. This is due to the presence of intrinsic defects, such as oxygen vacancy. However, in ZnO/Ag 5 min, a peak is formed in green shift region but the peak is not the same as the other peaks due to the concentration of Ag was different. It was concluded that the enhanced of the concentration of dopant Ag could affect the result of the emission and intensity. According to Zhang, emission of Ag peak at wavelength of 330 nm. Furthermore, Ag concentration addition into ZnO, ZnO/Ag will be red shift [34]. XRD spectrum was used to determine the crystal structure of colloid nanoparticles. XRD analysis of ZnO, ZnO/Ag and Ag nanoparticles is shown in Fig. 5. The result of ZnO nanoparticles shows all the peaks had a hexagonal wurtzite crystal structure, it because the structure of the results was almost the same as the previous study [31]. No other phase was observed which shows no inclusion of Zn in ZnO, which corresponds to the UV–Vis spectrum [35,36]. Based on the XRD results, ZnO peaks were detected at 31.79°, 34,52°, 36,24°, 47.73°, 56.56° and 62.81° with hkl values respectively (101), (002), (100), (102), (110), and (103). Ag peak is formed at 38.11°, 44.36°, 66.47° and 77.39° with hkl values in a row (111), (200), (220), and (311). The results were calculated by using Scherrer equation [31]:
Fig. 4. PL Spectra of Pure ZnO and Ag doped ZnO nanoparticles.
Fig. 5. XRD patterns of ZnO/Ag Nanoparticles. 3
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Fig. 6. TEM image and Particle Size Distribution of Pure ZnO (a) Pure Ag (b) ZnO/Ag 1 min (c) ZnO/Ag 3 min (d) ZnO/Ag 5 min (e).
4
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D=
0.9 λ β Cos θ
particle size is about 21 nm clearly. Acknowledgements
where D is the average crystal size (nm), λ = 1.54056 Å is the wavelength of the radiation., β is the width at half maximum intensity in radians at 2θ (°) and θ is Diffraction angle (Bragg Angle). Doping is a way to change the electrical and optical properties of semiconductors. One of the purposes of doping is to enhancement the conductivity of ZnO. Ag is an element that can be used as a dopant because it can be an absorber to collect photoelectrons that produced from ZnO conduction bands, it can be effective for inhibit electron-hole recombination [30]. Based on the XRD analysis results, the diffraction peaks were obtained on each ZnO nanoparticles which doped by Ag with doping time variations of 1 min, 3 min and 5 min. At ZnO/Ag 1 min peaks are formed at angle of 2θ: 28.13°, 31.78°, 34.43°, 36.22°, 47.65° with an average crystal size is 11.0577 nm. At ZnO/Ag 3 min, peaks are formed at angle of 2θ: 29.0°, 31.73°, 34.36°, 36,19°, 47.62° with an average crystal size is 14.7711 nm for ZnO/Ag 5 min, peaks are formed at angle of 2θ: 28.91°, 31.73°, 34.43°, 36.2°, 47.44° with an average crystal size is 10.6467 nm. From the results, peak Ag on ZnO doped at 2θ = 38.11° is invisible as shown in Fig. 5. It's because Ag+ ions behave as monovalent dopants, which have the ability to cover both lattices and interstitial sites because of high radius ion Ag+. The effect of combining Ag in the ZnO lattice was studied by monetizing the position and binding of the diffraction peak which is influenced by the level of operation due to the incorporation of Ag [32]. However, observed at angle of 2θ: 35°–37°, the peak shift occurs at angle of 36.0°–36.3°. Each enhancement of dopant concentration, the peak formed will lead to the left. It's indicates that Ag managed to be a dopant and not core/shell, the enhancement of Ag doesn't change the phase or lattice of ZnO nanoparticles and any enhancement of Ag to ZnO concentration also increases the intensity. Morphological analysis of ZnO, ZnO/Ag and Ag nanoparticles was tested by using TEM. The results show the morphological form of ZnO without Ag doping and after Ag dopant was shown in Fig. 6. The results show, the form of ZnO nanoparticles with a magnification of 50 nm are nanorods whereas the shape of Ag nanoparticles with the same magnification is sphere, which are shown in Fig. 6 (a) and (b). The color of Ag nanoparticles is dark predominantly than ZnO, it's because Ag has a large atomic number and the nanoparticles synthesis results shows, Ag colloid is more concentrated than ZnO colloid which tends to be grayish. After the enhancement of Ag dopant, transforms the structure, from nanorod structure to the sphere structure along with the enhancement of concentration as an effect of Ag doping in Fig. 6 (c), (d), and (e). It shows, if Ag is aggregate and there are several agglomeration points as the effect of Ag. In addition, agglomeration causes color differences. The darker color, indicates that more crystal is accumulated at each other at a certain point. Based on the TEM data analysis, the average ZnO and Ag nanoparticles is around 13–20 nm and 10–35 nm (see Fig. 6) which is due to be XRD analysis. Also, the average for ZnO doping Ag with 1, 3 and 5 min ablation is around 10–20 nm.
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