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Polyvinyl pyrrolidone blend for enhancement the electrical conductivity
Journal of Molecular Structure 1207 (2020) 127807
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Journal of Molecular Structure journal homepage: http://www.elsevier.com/locate/molstruc
Pulsed laser ablation route assisted copper oxide nanoparticles doped in Polyethylene Oxide/Polyvinyl pyrrolidone blend for enhancement the electrical conductivity A.A. Menazea Laser Technology Unit, National Research Centre, Spectroscopy Department, Physics Division, Dokki, 12311, Giza, Egypt
a r t i c l e i n f o
a b s t r a c t
Article history: Received 7 December 2019 Received in revised form 25 January 2020 Accepted 26 January 2020 Available online 27 January 2020
Polyethylene Oxide/Polyvinyl pyrrolidone blend was doped by Copper Oxide Nanoparticles (CuONPs) prepared by laser ablation process. Synthesized Copper oxide nanoparticles were prepared by ablating pure copper plate immersed in DDW by nanosecond Nd:YAG laser in different times. PEO/PVP/CuONPs nanocomposites have been synthesized via casting technique. Effect of CuONPs doping on enhancing PEO/PVP have been obtained. The influence of various times of laser ablation on the properties of the synthesized nanocomposite films was analyzed via several techniques. SEM and XRD proved the interaction between PEO/PVP blend and CuONPs. The presence of the distinctive absorption peak at UVeVis range at 277 nm was due to copper oxide surface plasmon resonance (SPR). The direct and indirect optical band gap values illustrate a decrease following doping of copper oxide inside PEO/PVP matrix. Dielectric constant and dielectric loss activity gradually diminished as the frequency rises. AC conductivity were increased as laser time increased. © 2020 Elsevier B.V. All rights reserved.
Keywords: Pulsed laser ablation PEO/PVP Copper oxide nanoparticles Ac conductivity
1. Introduction Nanomaterials have desirable characteristics which vary fundamentally with their mass state. Metal nanoparticles exhibit extraordinary physical, chemical, magnetic, antibacterial, electronic, and thermal properties [1e6]. CuONPs have a high priority through the metal nanoparticles, depending on their opportunity to interact essentially with light through effectively by dint of surface plasmon resonance (SPR) [7,8]. Due to their variety of applications, CuONPs have become very active in catalytic, electrical, optical, antibacterial, and mechanical properties [9e13]. Polyethylene oxide (PEO) is a linear, semi-crystalline polymer with high thermal and chemical strength [14]. A wide order of the crystalline structure phase of PEO polymer has verified its conductivity, and must therefore be coupled with amorphous polymer. The desirable characterization of polyvinyl pyrrolidone (PVP) is mechanical efficiency and excellent thermal stability and [15]. PVP is an efficient reducing agent for nanoparticles due to assist maintain metal NPs within its matrix due to the existence of carbonyl groups [16].
E-mail addresses: [email protected], [email protected]. https://doi.org/10.1016/j.molstruc.2020.127807 0022-2860/© 2020 Elsevier B.V. All rights reserved.
Polymer mixing is known to be one of the best ways to develop new polymeric products and grow materials with a wide range of properties [17]. The final result of the blending method can be adjusted to the needs of requirements that cannot be done by a single polymer. Composite of polymer/nanoparticles is actually have a great interest in introducing new ways to obtain a new substance with desirable properties that show benefits in terms of various properties [18e21]. Because of its fast processing capability and fair electrical conductivity in relation to its individual features, PVP was considered a good PEO collaborator in polymer mixing [22,23]. The pulsed laser ablation of solids in air [24,25] and liquids [26e28] assisted the synthesis of metal nanoparticles deemed an efficient route with major advantages over other routes. Pulsed Laser Ablation in Liquids (PLAL) route for synthesis metal nanoparticles promises new physical strategies to achieve metal colloids. PLAL method finds that a modern fantastic way to prepare large-quality nanoparticles from bulk metal has easy experimental setup [29e31]. This research was carried out to achieve the production of copper oxide nanoparticles in Double Distilled Water (DDW) by Nd:YAG laser ablation at different laser times; (5, 7.5, 10, 12.5, and 15 min). Then study the procedure of doping the prepared CuONPs
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in PEO/PVP by casting method in order to enhance the electrical characterization of PE/PVP blend. Ac conductivity of the prepared samples of PEO/PVP/CuONPs was carried out using A.C as a function of frequency in room temperature measurements. 2. Materials and method 2.1. Materials PEO with molecular weight M.W. z 40,000 g/mol was purchased from Sigma Aldrich in powder form and PVP with M.W. z 72,000 g/mol was purchased from ACROS in powder form. Both PEO and PVP polymers were used as basic components of the polymeric blend. Double Distilled Water (DDW) was used as a common solvent for each PEO and PVP. Copper plate was purchased with high purity of (99.999%). 2.2. Preparation of copper oxide nanoparticles Copper oxide nanoparticles were prepared by laser ablation process. The experimental setup of generation of nanoparticles by PLAL was described previously in details [26]. Nd:YAG pulsed nanosecond laser at 1064 nm was utilized as source of ablation
Fig. 1. XRD patterns of (a) pure PEO and pure PVP and (b) pure PEO/PVP blend and PEO/PVP/CuONPs composites.
process. The laser source has 3.6 W powers, 10 Hz pulse repetition rate, 7 nm pulse duration. Copper metal plate (4 mm radius 3 mm thickness) was polished with emery paper and washed several times in DDW. The copper plate was immersed in a vessel’s bottom containing 30 ml of DDW. The thickness of DDW above the target was about 7 mm. The laser beam was focused perpendicularly on the copper plate by a lens with a focal length of 10 cm to enable the laser ablation on the surface. The laser ablation process was repeated different times by different laser ablation time; (5, 7.5, 10, 12.5, and 15 min).
2.3. Preparation of PEO/PVP/CuONPs composite 0.77 g of PEO and 0.33 g of PVP in powder form was added and dissolved in 30 ml of the prepared copper oxide nanoparticles with continuous stirring for 21 h at 50 C to complete the dissolution process until homogenous viscous liquid slurry was established. This step was repeated for all the prepared copper oxide nanoparticles at different time laser ablation, separately. The prepared films of PEO/PVP/CuONPs nanocomposite were formed via solution
Fig. 2. (a) UVeVisible absorption spectra, (b) plots of absorption coefficient (a) versus (hʋ) of pure PEO/PVP blend and PEO/PVP/CuONPs composites.
A.A. Menazea / Journal of Molecular Structure 1207 (2020) 127807
casting technique; the solution of each laser ablation time was poured into polypropylene dishes and dried in the furnace at 40 C for 5 days. After drying process, the prepared films at the bottom of dishes were stripped off from the dishes and placed in heavily evacuated desiccators to avoid the absorption of moisture. The thickness of prepared films was in the range of 0.2 mm. 2.4. Characterization techniques XRD scans were obtained via (Schimadzu 7000, Japan) occupied with Cu-Ka radiation (l ¼ 0.154060 nm) generated at 30 kV and 30 mA, diffraction patterns were collected within the Bragg’s angle (2q) ranging between 5 and 80 . UVeVisible spectroscopy analysis was performed via JASCO (V-570) double beam spectrophotometer in the wavelength region of 200e1000 nm at room temperature. Surface morphology of the samples was examined via a Field Emission-Scanning Electron Microscope (FE-SEM) type (Quanta FEG 250, USA). AC conductivity measurements were carried out by using The Broadband Dielectric Spectroscopy (BDS) type (concept 40) Novocontrol High Resolution Alpha Analyzer assisted by Quatro Temperature Controllers using pure nitrogen as the heating agent. The samples were measured at room temperature in frequency range from 0.1 Hz to 20 MHz. 3. Results and discussion 3.1. X-ray diffraction analysis (XRD) XRD scans of both PEO and PVP was illustrated in Fig. 1.a. XRD scans in PEO spectrum reflects PEO’s semi-crystalline nature and displays peaks at 2q: 19 , 23 which 26 attributed respectively to (112), (120) and (222) [32]. The PEO spectrum also recorded many low intensity peaks near 2q: 12 , 14 , 28 , 30 , 36 , 39 and 44 . XRD scans in PVP spectrum reflects PEO’s amorphous nature and displays peaks at 10 and 21 [33]. Fig. 1. b shows the XRD scans of the PEO/PVP blend and copper nanoparticles doped blend at various times of laser ablation. XRD scans of pure PEO/PVP film
3
shows two peaks at 2q; 19 and 23 and also show low strong peaks at 2q: 14 , 27, 30 and 36 related to PEO existence and reveal the semi-crystalline of blend structure. The XRD spectrum of PEO/PVP/ CuONPs composite films results in a rise in the strength of the two major diffraction peaks 19 and 23 in low doping, then decrease in intensity from 7.5 min with an improvement in laser ablation time up to high doping. The intensity of peaks is also declining at 14 , 27, with the laser ablation time raising. This reduction implies that the arrangement of CuONPs in the blend is now unexpected and leads to a decrease in the degree of crystallinity and this can confirm the complexation between copper oxide nanoparticles and blend. In addition, XRD scans of nanocomposite shows the distinctive sharp diffraction peak at 2 ¼ 38 attributing to the plane (111) indexed for single-phase of copper oxide nanoparticles with a monoclinical structure (JCPDS File No. 05e661) [34]. The disappearance of the most peaks of copper oxide nanoparticles could be attributed to the low doping in PEO/PVP system by CuONPs prepared by laser ablation. Fig. 1. b indicates a rise in intensity of peak shows that the amount of copper oxide nanoparticles in the blend mixture increased by growing the duration of laser ablation. The crystalline size of copper oxide nanoparticles was determined using Debye- Scherrer’s equation [35]:
size ¼ kl=bCosq
(1)
According the formula, the average size of doped copper oxide nanoparticles in PEO/PVP at 2q ¼ 38 is ranged between 18 nm and 34 nm. These values suggest that the size of copper oxide nanoparticles increased after the doping process within the PEO/PVP matrix which was confirmed by UVeVis analysis. 3.2. Optical properties (UVeVis) Fig. 2.a indicates the absorption spectrum of pure PEO/PVP and PEO/PVP blend doped with copper oxide nanoparticles nanocomposites prepared at different laser ablation time. Pure PEO/PVP demonstrates the only absorption peak in the UV spectrum that
Fig. 3. FE-SEM photos of PEO/PVP doped by copper oxide nanoparticles prepared at different laser ablation time; (a) 5 min, (b) 10 min, and (c) 15 min.
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appeared at 207 nm, which can be ascribed primarily to n/p* electronic transitions and there are no peaks in within the range 300e600 nm confirming the semi-crystalline structure [36]. UVeVis spectra of PEO/PVP blend embedded with CuONPs that prepared at various laser ablation times illustrate a red shift for the peak that located at 207 nm that approved the interaction between PEO/PVP matrix and copper oxide nanoparticles. PEO/PVP/CuONPs UVeVis absorption spectrum in Fig. 2. a reaches a significant absorption peak of 277 nm that assigned to SPR of copper oxide nanoparticles [37] and approved the doped copper oxide nanoparticles inside PEO/PVP blend. With increasing the times of laser ablation, the embedded copper oxide in the PEO/PVP matrix increased and the peak strength of the SPR increased [38]. Also, in this case, the nanocomposite sample chains are believed to be interlinked with others, leading to enhance the amorphous content. Furthermore, the decrease in SPR peak broadness suggests that the narrow size distribution of CuONPs at higher laser ablation time. Optical absorption coefficients a of pure PEO/PVP and PEO/PVP blend doped with copper oxide nanoparticles nanocomposites samples were illustrated in Fig. 2. b as a function in wavelength l and can be determined via BeereLambert’s equation [39]:
a ðlÞ ¼
2:303 A d
20 MHz).
3.4.1. Dielectric analysis Fig. 4 (a and b) reflect the frequencies dependency for the prepared samples on the dielectric constant ε0 and the dielectric loss ε" for the synthesized samples. The complex dielectric of a material was given according to Debye as the formula [41]:
ε ¼ ε0 þ j ε〞
(5)
The values of ε0 and ε’’ of the pure blend at high frequencies are small and when embedded by copper oxide nanoparticles, these values have been increased as the doping in the blend increased then it reached a constant value at high frequencies that due to polarization effects [42]. The dielectric losses can calculate by the formula: 00
ε ¼ ε0 tand
(6)
(2)
By increasing the times of laser ablation, absorption edge has been shifted to lower photon energy, a is increased. From this, we can say that the optical band gap of pure blend have been decreased after embedded with CuONPs. The absorption edge value of pure blend is 4.55 eV, but decreased dramatically by growing the times of laser ablation to 3.28 eV for the blend embedded by copper oxide nanoparticles at high value of time. The optical band gap Eg could be directly measure via Tauc’s equation [40]:
ahy ¼ A hy Eg
m
(3)
3.3. Field Emission-Scanning Electron Microscope (SEM) FE-SEM has been conducted to demonstrate the modifications arising from the embedded copper oxide nanoparticles to the PEO/ PVP surface. Fig. 3 illustrate FE-SEM micrographs of pure blend doped by CuONPs at various times of laser ablation for 5, 10, and 15 min. In Fig. 3(aec), FE-SEM micrographs of PEO/PVP doped with copper oxide nanoparticles obtain an arising of the embedded copper oxide nanoparticles on the surface of the sample by increasing the time of laser ablation. Fig. 4.a shows a white amount of bright copper nanoparticles with the finest arrangement on the sample surface for laser ablation time 5 min. With raising the laser ablation time to 10 min in Fig. 3. b, we have seen that many agglomerates that started to be obtained in certain sections of the sample. Fig. 3. c for 15 min, the copper oxide nanoparticles were aggregates and acquired as large granules and acquired as bright spots. The copper oxide nanoparticles were incorporated bit by bit into the blend with growing the times of laser ablation. These results illustrate the complexation process between copper oxide nanoparticles and PEO/PVP matrix. 3.4. AC electrical conductivity Ac conductivity and the dielectric properties of the synthesized pure blend and after embedded via copper oxide nanoparticles at various times of ablation time have been evaluated at room temperature as a function of the frequency in the range (0.1 Hz -
Fig. 4. Typical plots of variation of (a) real part (ε0 ) and (b) imaginary part (ε’’) of the dielectric constant with frequency for pure PEO/PVP blend and PEO/PVP/CuONPs composites.
A.A. Menazea / Journal of Molecular Structure 1207 (2020) 127807
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3.4.2. Conductivity analysis fig. 5 (a and b) obtains the real sac’ and imaginary sac’’ part of conductivity as a function in frequency (log f). Values of sac’ are very small at low frequencies then begin to increase as the frequencies increased. This increasing may be attributed to spacecharge polarization [43]. These values have been increased as the concentrations of copper oxide nanoparticles increased in the blend at higher frequencies. Values of sac’’ are very high at low frequencies begin to decrease as the frequency increased.
3.4.3. Complex impedance analysis fig. 6 (a and b) shows the real Z0 and imaginary Z00 part of impedance in dependence of frequency (log f). Ac-impedance complex Z could be obtained by the formula [44]: 00
Z ¼ Z’ þ j Z
(10) Z0
and Z00
Values of are very high at low frequencies then it begin to deceasing by the frequency increased. This increasing is continuing until it exceeded constant values at the higher frequencies. We can found that the values of Z0 and Z00 at low frequencies are increased as the laser ablation time increased.
Fig. 6. Typical plots of variation of (a) real part (Z0 ) and (b) imaginary part (Z00 ) of the electric impedance with frequency for pure PEO/PVP blend and PEO/PVP/CuONPs composites.
4. Conclusion
Fig. 5. Typical plots of variation of (a) real part (sac’) and (b) imaginary part (sac’’) of the total conductivity with frequency for pure PEO/PVP blend and PEO/PVP/CuONPs composites.
In this study, Nd:YAG laser was used to production copper oxide nanoparticles at different ablation time. The prepared CuONPs was used to form PEO/PVP/CuONPs via casting method. The role of CuONPs has been studied in enhancing the electrical conductivity of PEO/PVP. XRD achieves the characteristic diffraction peak of CuONPs at 2q ¼ 38 which confirm the embedded copper oxide nanoparticles. Reports of optical observations suggest great potential in photonics and optoelectronics applications of the CuONPs doped in PEO/PVP blend. FE-SEM photos obtain a significant difference in the surface properties of the synthesized samples which confirms the surface embedded by copper oxide nanoparticles. Values of ε0 and ε’’ have been increased as the times of laser ablation values were increased with increase the laser ablation time, as well as a decrease in the values hitting the constant values at higher frequencies. The values of Z0 and Z00 at low frequencies are increased by increasing the embedded copper oxide nanoparticles in the PEO/ PVP blend matrix.
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Pulsed laser ablation route assisted copper oxide nanoparticles doped in Polyethylene Oxide/Polyvinyl pyrrolidone blend for enhancement the electrical conductivity A.A. Menazea Laser Technology Unit, National Research Centre, Spectroscopy Department, Physics Division, Dokki, 12311, Giza, Egypt
a r t i c l e i n f o
a b s t r a c t
Article history: Received 7 December 2019 Received in revised form 25 January 2020 Accepted 26 January 2020 Available online 27 January 2020
Polyethylene Oxide/Polyvinyl pyrrolidone blend was doped by Copper Oxide Nanoparticles (CuONPs) prepared by laser ablation process. Synthesized Copper oxide nanoparticles were prepared by ablating pure copper plate immersed in DDW by nanosecond Nd:YAG laser in different times. PEO/PVP/CuONPs nanocomposites have been synthesized via casting technique. Effect of CuONPs doping on enhancing PEO/PVP have been obtained. The influence of various times of laser ablation on the properties of the synthesized nanocomposite films was analyzed via several techniques. SEM and XRD proved the interaction between PEO/PVP blend and CuONPs. The presence of the distinctive absorption peak at UVeVis range at 277 nm was due to copper oxide surface plasmon resonance (SPR). The direct and indirect optical band gap values illustrate a decrease following doping of copper oxide inside PEO/PVP matrix. Dielectric constant and dielectric loss activity gradually diminished as the frequency rises. AC conductivity were increased as laser time increased. © 2020 Elsevier B.V. All rights reserved.
Keywords: Pulsed laser ablation PEO/PVP Copper oxide nanoparticles Ac conductivity
1. Introduction Nanomaterials have desirable characteristics which vary fundamentally with their mass state. Metal nanoparticles exhibit extraordinary physical, chemical, magnetic, antibacterial, electronic, and thermal properties [1e6]. CuONPs have a high priority through the metal nanoparticles, depending on their opportunity to interact essentially with light through effectively by dint of surface plasmon resonance (SPR) [7,8]. Due to their variety of applications, CuONPs have become very active in catalytic, electrical, optical, antibacterial, and mechanical properties [9e13]. Polyethylene oxide (PEO) is a linear, semi-crystalline polymer with high thermal and chemical strength [14]. A wide order of the crystalline structure phase of PEO polymer has verified its conductivity, and must therefore be coupled with amorphous polymer. The desirable characterization of polyvinyl pyrrolidone (PVP) is mechanical efficiency and excellent thermal stability and [15]. PVP is an efficient reducing agent for nanoparticles due to assist maintain metal NPs within its matrix due to the existence of carbonyl groups [16].
E-mail addresses: [email protected], [email protected]. https://doi.org/10.1016/j.molstruc.2020.127807 0022-2860/© 2020 Elsevier B.V. All rights reserved.
Polymer mixing is known to be one of the best ways to develop new polymeric products and grow materials with a wide range of properties [17]. The final result of the blending method can be adjusted to the needs of requirements that cannot be done by a single polymer. Composite of polymer/nanoparticles is actually have a great interest in introducing new ways to obtain a new substance with desirable properties that show benefits in terms of various properties [18e21]. Because of its fast processing capability and fair electrical conductivity in relation to its individual features, PVP was considered a good PEO collaborator in polymer mixing [22,23]. The pulsed laser ablation of solids in air [24,25] and liquids [26e28] assisted the synthesis of metal nanoparticles deemed an efficient route with major advantages over other routes. Pulsed Laser Ablation in Liquids (PLAL) route for synthesis metal nanoparticles promises new physical strategies to achieve metal colloids. PLAL method finds that a modern fantastic way to prepare large-quality nanoparticles from bulk metal has easy experimental setup [29e31]. This research was carried out to achieve the production of copper oxide nanoparticles in Double Distilled Water (DDW) by Nd:YAG laser ablation at different laser times; (5, 7.5, 10, 12.5, and 15 min). Then study the procedure of doping the prepared CuONPs
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in PEO/PVP by casting method in order to enhance the electrical characterization of PE/PVP blend. Ac conductivity of the prepared samples of PEO/PVP/CuONPs was carried out using A.C as a function of frequency in room temperature measurements. 2. Materials and method 2.1. Materials PEO with molecular weight M.W. z 40,000 g/mol was purchased from Sigma Aldrich in powder form and PVP with M.W. z 72,000 g/mol was purchased from ACROS in powder form. Both PEO and PVP polymers were used as basic components of the polymeric blend. Double Distilled Water (DDW) was used as a common solvent for each PEO and PVP. Copper plate was purchased with high purity of (99.999%). 2.2. Preparation of copper oxide nanoparticles Copper oxide nanoparticles were prepared by laser ablation process. The experimental setup of generation of nanoparticles by PLAL was described previously in details [26]. Nd:YAG pulsed nanosecond laser at 1064 nm was utilized as source of ablation
Fig. 1. XRD patterns of (a) pure PEO and pure PVP and (b) pure PEO/PVP blend and PEO/PVP/CuONPs composites.
process. The laser source has 3.6 W powers, 10 Hz pulse repetition rate, 7 nm pulse duration. Copper metal plate (4 mm radius 3 mm thickness) was polished with emery paper and washed several times in DDW. The copper plate was immersed in a vessel’s bottom containing 30 ml of DDW. The thickness of DDW above the target was about 7 mm. The laser beam was focused perpendicularly on the copper plate by a lens with a focal length of 10 cm to enable the laser ablation on the surface. The laser ablation process was repeated different times by different laser ablation time; (5, 7.5, 10, 12.5, and 15 min).
2.3. Preparation of PEO/PVP/CuONPs composite 0.77 g of PEO and 0.33 g of PVP in powder form was added and dissolved in 30 ml of the prepared copper oxide nanoparticles with continuous stirring for 21 h at 50 C to complete the dissolution process until homogenous viscous liquid slurry was established. This step was repeated for all the prepared copper oxide nanoparticles at different time laser ablation, separately. The prepared films of PEO/PVP/CuONPs nanocomposite were formed via solution
Fig. 2. (a) UVeVisible absorption spectra, (b) plots of absorption coefficient (a) versus (hʋ) of pure PEO/PVP blend and PEO/PVP/CuONPs composites.
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casting technique; the solution of each laser ablation time was poured into polypropylene dishes and dried in the furnace at 40 C for 5 days. After drying process, the prepared films at the bottom of dishes were stripped off from the dishes and placed in heavily evacuated desiccators to avoid the absorption of moisture. The thickness of prepared films was in the range of 0.2 mm. 2.4. Characterization techniques XRD scans were obtained via (Schimadzu 7000, Japan) occupied with Cu-Ka radiation (l ¼ 0.154060 nm) generated at 30 kV and 30 mA, diffraction patterns were collected within the Bragg’s angle (2q) ranging between 5 and 80 . UVeVisible spectroscopy analysis was performed via JASCO (V-570) double beam spectrophotometer in the wavelength region of 200e1000 nm at room temperature. Surface morphology of the samples was examined via a Field Emission-Scanning Electron Microscope (FE-SEM) type (Quanta FEG 250, USA). AC conductivity measurements were carried out by using The Broadband Dielectric Spectroscopy (BDS) type (concept 40) Novocontrol High Resolution Alpha Analyzer assisted by Quatro Temperature Controllers using pure nitrogen as the heating agent. The samples were measured at room temperature in frequency range from 0.1 Hz to 20 MHz. 3. Results and discussion 3.1. X-ray diffraction analysis (XRD) XRD scans of both PEO and PVP was illustrated in Fig. 1.a. XRD scans in PEO spectrum reflects PEO’s semi-crystalline nature and displays peaks at 2q: 19 , 23 which 26 attributed respectively to (112), (120) and (222) [32]. The PEO spectrum also recorded many low intensity peaks near 2q: 12 , 14 , 28 , 30 , 36 , 39 and 44 . XRD scans in PVP spectrum reflects PEO’s amorphous nature and displays peaks at 10 and 21 [33]. Fig. 1. b shows the XRD scans of the PEO/PVP blend and copper nanoparticles doped blend at various times of laser ablation. XRD scans of pure PEO/PVP film
3
shows two peaks at 2q; 19 and 23 and also show low strong peaks at 2q: 14 , 27, 30 and 36 related to PEO existence and reveal the semi-crystalline of blend structure. The XRD spectrum of PEO/PVP/ CuONPs composite films results in a rise in the strength of the two major diffraction peaks 19 and 23 in low doping, then decrease in intensity from 7.5 min with an improvement in laser ablation time up to high doping. The intensity of peaks is also declining at 14 , 27, with the laser ablation time raising. This reduction implies that the arrangement of CuONPs in the blend is now unexpected and leads to a decrease in the degree of crystallinity and this can confirm the complexation between copper oxide nanoparticles and blend. In addition, XRD scans of nanocomposite shows the distinctive sharp diffraction peak at 2 ¼ 38 attributing to the plane (111) indexed for single-phase of copper oxide nanoparticles with a monoclinical structure (JCPDS File No. 05e661) [34]. The disappearance of the most peaks of copper oxide nanoparticles could be attributed to the low doping in PEO/PVP system by CuONPs prepared by laser ablation. Fig. 1. b indicates a rise in intensity of peak shows that the amount of copper oxide nanoparticles in the blend mixture increased by growing the duration of laser ablation. The crystalline size of copper oxide nanoparticles was determined using Debye- Scherrer’s equation [35]:
size ¼ kl=bCosq
(1)
According the formula, the average size of doped copper oxide nanoparticles in PEO/PVP at 2q ¼ 38 is ranged between 18 nm and 34 nm. These values suggest that the size of copper oxide nanoparticles increased after the doping process within the PEO/PVP matrix which was confirmed by UVeVis analysis. 3.2. Optical properties (UVeVis) Fig. 2.a indicates the absorption spectrum of pure PEO/PVP and PEO/PVP blend doped with copper oxide nanoparticles nanocomposites prepared at different laser ablation time. Pure PEO/PVP demonstrates the only absorption peak in the UV spectrum that
Fig. 3. FE-SEM photos of PEO/PVP doped by copper oxide nanoparticles prepared at different laser ablation time; (a) 5 min, (b) 10 min, and (c) 15 min.
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appeared at 207 nm, which can be ascribed primarily to n/p* electronic transitions and there are no peaks in within the range 300e600 nm confirming the semi-crystalline structure [36]. UVeVis spectra of PEO/PVP blend embedded with CuONPs that prepared at various laser ablation times illustrate a red shift for the peak that located at 207 nm that approved the interaction between PEO/PVP matrix and copper oxide nanoparticles. PEO/PVP/CuONPs UVeVis absorption spectrum in Fig. 2. a reaches a significant absorption peak of 277 nm that assigned to SPR of copper oxide nanoparticles [37] and approved the doped copper oxide nanoparticles inside PEO/PVP blend. With increasing the times of laser ablation, the embedded copper oxide in the PEO/PVP matrix increased and the peak strength of the SPR increased [38]. Also, in this case, the nanocomposite sample chains are believed to be interlinked with others, leading to enhance the amorphous content. Furthermore, the decrease in SPR peak broadness suggests that the narrow size distribution of CuONPs at higher laser ablation time. Optical absorption coefficients a of pure PEO/PVP and PEO/PVP blend doped with copper oxide nanoparticles nanocomposites samples were illustrated in Fig. 2. b as a function in wavelength l and can be determined via BeereLambert’s equation [39]:
a ðlÞ ¼
2:303 A d
20 MHz).
3.4.1. Dielectric analysis Fig. 4 (a and b) reflect the frequencies dependency for the prepared samples on the dielectric constant ε0 and the dielectric loss ε" for the synthesized samples. The complex dielectric of a material was given according to Debye as the formula [41]:
ε ¼ ε0 þ j ε〞
(5)
The values of ε0 and ε’’ of the pure blend at high frequencies are small and when embedded by copper oxide nanoparticles, these values have been increased as the doping in the blend increased then it reached a constant value at high frequencies that due to polarization effects [42]. The dielectric losses can calculate by the formula: 00
ε ¼ ε0 tand
(6)
(2)
By increasing the times of laser ablation, absorption edge has been shifted to lower photon energy, a is increased. From this, we can say that the optical band gap of pure blend have been decreased after embedded with CuONPs. The absorption edge value of pure blend is 4.55 eV, but decreased dramatically by growing the times of laser ablation to 3.28 eV for the blend embedded by copper oxide nanoparticles at high value of time. The optical band gap Eg could be directly measure via Tauc’s equation [40]:
ahy ¼ A hy Eg
m
(3)
3.3. Field Emission-Scanning Electron Microscope (SEM) FE-SEM has been conducted to demonstrate the modifications arising from the embedded copper oxide nanoparticles to the PEO/ PVP surface. Fig. 3 illustrate FE-SEM micrographs of pure blend doped by CuONPs at various times of laser ablation for 5, 10, and 15 min. In Fig. 3(aec), FE-SEM micrographs of PEO/PVP doped with copper oxide nanoparticles obtain an arising of the embedded copper oxide nanoparticles on the surface of the sample by increasing the time of laser ablation. Fig. 4.a shows a white amount of bright copper nanoparticles with the finest arrangement on the sample surface for laser ablation time 5 min. With raising the laser ablation time to 10 min in Fig. 3. b, we have seen that many agglomerates that started to be obtained in certain sections of the sample. Fig. 3. c for 15 min, the copper oxide nanoparticles were aggregates and acquired as large granules and acquired as bright spots. The copper oxide nanoparticles were incorporated bit by bit into the blend with growing the times of laser ablation. These results illustrate the complexation process between copper oxide nanoparticles and PEO/PVP matrix. 3.4. AC electrical conductivity Ac conductivity and the dielectric properties of the synthesized pure blend and after embedded via copper oxide nanoparticles at various times of ablation time have been evaluated at room temperature as a function of the frequency in the range (0.1 Hz -
Fig. 4. Typical plots of variation of (a) real part (ε0 ) and (b) imaginary part (ε’’) of the dielectric constant with frequency for pure PEO/PVP blend and PEO/PVP/CuONPs composites.
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3.4.2. Conductivity analysis fig. 5 (a and b) obtains the real sac’ and imaginary sac’’ part of conductivity as a function in frequency (log f). Values of sac’ are very small at low frequencies then begin to increase as the frequencies increased. This increasing may be attributed to spacecharge polarization [43]. These values have been increased as the concentrations of copper oxide nanoparticles increased in the blend at higher frequencies. Values of sac’’ are very high at low frequencies begin to decrease as the frequency increased.
3.4.3. Complex impedance analysis fig. 6 (a and b) shows the real Z0 and imaginary Z00 part of impedance in dependence of frequency (log f). Ac-impedance complex Z could be obtained by the formula [44]: 00
Z ¼ Z’ þ j Z
(10) Z0
and Z00
Values of are very high at low frequencies then it begin to deceasing by the frequency increased. This increasing is continuing until it exceeded constant values at the higher frequencies. We can found that the values of Z0 and Z00 at low frequencies are increased as the laser ablation time increased.
Fig. 6. Typical plots of variation of (a) real part (Z0 ) and (b) imaginary part (Z00 ) of the electric impedance with frequency for pure PEO/PVP blend and PEO/PVP/CuONPs composites.
4. Conclusion
Fig. 5. Typical plots of variation of (a) real part (sac’) and (b) imaginary part (sac’’) of the total conductivity with frequency for pure PEO/PVP blend and PEO/PVP/CuONPs composites.
In this study, Nd:YAG laser was used to production copper oxide nanoparticles at different ablation time. The prepared CuONPs was used to form PEO/PVP/CuONPs via casting method. The role of CuONPs has been studied in enhancing the electrical conductivity of PEO/PVP. XRD achieves the characteristic diffraction peak of CuONPs at 2q ¼ 38 which confirm the embedded copper oxide nanoparticles. Reports of optical observations suggest great potential in photonics and optoelectronics applications of the CuONPs doped in PEO/PVP blend. FE-SEM photos obtain a significant difference in the surface properties of the synthesized samples which confirms the surface embedded by copper oxide nanoparticles. Values of ε0 and ε’’ have been increased as the times of laser ablation values were increased with increase the laser ablation time, as well as a decrease in the values hitting the constant values at higher frequencies. The values of Z0 and Z00 at low frequencies are increased by increasing the embedded copper oxide nanoparticles in the PEO/ PVP blend matrix.
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