Synthesis and characterization of CdSe quantum dots for solar cell application
- Authors: Makinana, Sinovuyo
- Date: 2017
- Subjects: Quantum dots Quantum dots -- Optical properties Renewable energy sources
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: http://hdl.handle.net/10353/5994 , vital:29466
- Description: This study shows a detailed report on the morphological, structural and optical properties of CdSe QDs synthesised by the hot injection method. Cadmium acetate dihydrate and Se powder were used as cadmium and selenide precursors, respectively. Various QD sizes were achieved by synthesizing in temperature range of 150ºC, 175ºC, 200ºC, 225ºC, 250ºC, 275ºC and 300ºC, respectively. The as synthesized QDs by the hot injection method were cross-examined for their morphological, structural and optical using HRTEM, FTIR, XRD, RS, and UV-Vis spectroscopy techniques respectively. FTIR analysis has revealed vibrations at 738, 738, 738, 738, 735, 735 and 733 cm-1 for the QDs synthesized at various temperatures of 150, 175, 200, 225, 250, 275, and 300℃, respectively. The presence of the above mentioned peaks confirms the presence of Cd-Se bond in our samples. XRD analysis of CdSe QDs revealed diffraction peaks at 2 angles of 16.66 , 25.20 , 34.77 , 40.9 , 45.39 and 49.1 for 150 17.4 , 25.22 , 34.85 , 41.7 , 44.45 and 47.5 for the QDs synthesized at various temperatures of 175 17.07 , 25.19 , 34.85 , 41.34 , 44.41 and 48.86 for 200 ; 16.34 , 25.20 , 34.76 , 40.6 , 44.74 and 49.48 for 225 ; 17.44 , 25.17 , 34.19 , 41.7 , 44.45 , 49.24 for 250 ; 16.70 , 25.16 , 34.85 , 40.32 , 45.1 and 49.1 7 for 275 ;and 17.35 , 25.18 , 35.13 , 41.63 , 45.7 , 49.48 for 300 . These XRD peaks relate to crystal planes of (100), (002), (102), (220), (103) and (112) which belong to hexagonal Wurtzite CdSe crystal structure. Additionally XRD analysis has revealed a general peak shift to higher 2 values was observed for CdSe QDs. HRTEM analysis showed that the synthesised CdSe QDs have a spherical shape and are monodispersed. Moreover, HRTEM analysis has revealed CdSe QDs modal crystallite size of 1.79 nm, 1.81 nm, 2.06 nm, 2.08 nm, 2.11 nm, 3.10 nm and 3.12 nm for the QDs synthesized at various temperatures of 150ºC, 175ºC, 200ºC, 225ºC, 250ºC, 275ºC and 300ºC, respectively. HRTEM results were in mutual agreement with XRD results. Additionally, the SAED images showed intense electron diffraction rings, which confirmed that the as-synthesised CdSe QDs have a Wurtzite crystal structure. RS analysis showed that CdSe QDs have LO and 2LO vibrational modes which are characteristic peaks for CdSe. The presence of these peaks in Raman spectra further supports our previous observation from XRD analysis and HRTEM analysis that the synthesized CdSe QDs have a Wurtzite crystal structure. The effect of synthesis temperature Raman peak shift, FHWH and peak intensity has been cross examined in this work, Moreover, the effect of increasing temperature on the peak shift, FWHM and peak intensity is discussed in detail below. UV-Vis analysis revealed an absorbance of CdSe QDs in higher wavelengths as temperature was increased. Furthermore, the Yu et al 2003 relation was used to calculate QD size and band gap energy of CdSe QDs. The results showed that QD size increases with increasing synthesis temperature, which is in agreement with HRTEM and XRD results.
- Full Text:
- Authors: Makinana, Sinovuyo
- Date: 2017
- Subjects: Quantum dots Quantum dots -- Optical properties Renewable energy sources
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: http://hdl.handle.net/10353/5994 , vital:29466
- Description: This study shows a detailed report on the morphological, structural and optical properties of CdSe QDs synthesised by the hot injection method. Cadmium acetate dihydrate and Se powder were used as cadmium and selenide precursors, respectively. Various QD sizes were achieved by synthesizing in temperature range of 150ºC, 175ºC, 200ºC, 225ºC, 250ºC, 275ºC and 300ºC, respectively. The as synthesized QDs by the hot injection method were cross-examined for their morphological, structural and optical using HRTEM, FTIR, XRD, RS, and UV-Vis spectroscopy techniques respectively. FTIR analysis has revealed vibrations at 738, 738, 738, 738, 735, 735 and 733 cm-1 for the QDs synthesized at various temperatures of 150, 175, 200, 225, 250, 275, and 300℃, respectively. The presence of the above mentioned peaks confirms the presence of Cd-Se bond in our samples. XRD analysis of CdSe QDs revealed diffraction peaks at 2 angles of 16.66 , 25.20 , 34.77 , 40.9 , 45.39 and 49.1 for 150 17.4 , 25.22 , 34.85 , 41.7 , 44.45 and 47.5 for the QDs synthesized at various temperatures of 175 17.07 , 25.19 , 34.85 , 41.34 , 44.41 and 48.86 for 200 ; 16.34 , 25.20 , 34.76 , 40.6 , 44.74 and 49.48 for 225 ; 17.44 , 25.17 , 34.19 , 41.7 , 44.45 , 49.24 for 250 ; 16.70 , 25.16 , 34.85 , 40.32 , 45.1 and 49.1 7 for 275 ;and 17.35 , 25.18 , 35.13 , 41.63 , 45.7 , 49.48 for 300 . These XRD peaks relate to crystal planes of (100), (002), (102), (220), (103) and (112) which belong to hexagonal Wurtzite CdSe crystal structure. Additionally XRD analysis has revealed a general peak shift to higher 2 values was observed for CdSe QDs. HRTEM analysis showed that the synthesised CdSe QDs have a spherical shape and are monodispersed. Moreover, HRTEM analysis has revealed CdSe QDs modal crystallite size of 1.79 nm, 1.81 nm, 2.06 nm, 2.08 nm, 2.11 nm, 3.10 nm and 3.12 nm for the QDs synthesized at various temperatures of 150ºC, 175ºC, 200ºC, 225ºC, 250ºC, 275ºC and 300ºC, respectively. HRTEM results were in mutual agreement with XRD results. Additionally, the SAED images showed intense electron diffraction rings, which confirmed that the as-synthesised CdSe QDs have a Wurtzite crystal structure. RS analysis showed that CdSe QDs have LO and 2LO vibrational modes which are characteristic peaks for CdSe. The presence of these peaks in Raman spectra further supports our previous observation from XRD analysis and HRTEM analysis that the synthesized CdSe QDs have a Wurtzite crystal structure. The effect of synthesis temperature Raman peak shift, FHWH and peak intensity has been cross examined in this work, Moreover, the effect of increasing temperature on the peak shift, FWHM and peak intensity is discussed in detail below. UV-Vis analysis revealed an absorbance of CdSe QDs in higher wavelengths as temperature was increased. Furthermore, the Yu et al 2003 relation was used to calculate QD size and band gap energy of CdSe QDs. The results showed that QD size increases with increasing synthesis temperature, which is in agreement with HRTEM and XRD results.
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Synthesis of modified zinc oxide nanoparticles using pneumatic spray pyrolysis for solar cell application
- Authors: Ntozakhe, Luyolo
- Date: 2017
- Subjects: Zinc oxide -- Synthesis Nanoparticles
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: http://hdl.handle.net/10353/5862 , vital:29408
- Description: In this work, the pneumatic spray pyrolysis was used to synthesize un-doped and carbon doped zinc oxide (ZnO) nanoparticles. The zinc acetate, tetrabutylammonium bromide and ethanol were used as starting materials for the desired ZnO nanoparticles and the prepared samples were annealed at 400 oC in the furnace. The as synthesized un-doped and carbon doped ZnO NPs were evaluated using X-ray diffraction (XRD), Scanning electron microscope (SEM), Energy dispersive x-ray spectroscopy (EDX), High-resolution transmission electron microscopy (HRTEM), Raman spectroscopy (RS) and Ultraviolet-visible spectroscopy (UV-Vis). XRD analysis of the synthesized NPs revealed peaks at 31.90°, 34.50°, 36.34°, 47.73°, 56.88°, 63.04°, 68.20°, and 77.33° belonging to the hexagonal Wurtzite ZnO crystal structure. The incorporation of C species into ZnO lattice was cross examined by monitoring the peak positions of the (100), (002) and (001) planes. These three main peaks of C-ZnO NPs show a peak shift to higher 2θ values which indicates substitutional carbon doping in ZnO NPs. SEM analysis has revealed that the as synthesized NPs have spherical shape and the morphology of the NPs change as the concentration of carbon increases. The EDX spectra of both un-doped and doped ZnO nanoparticles have revealed prominent peaks at 0.51 keV, 1.01 keV, 1.49 keV, 8.87 keV and 9.86 keV. Peaks at, X-ray energies of 0.51 keV and 1.01 keV respectively represent the emissions from the K-shell of oxygen and L-shell of zinc. The L-shell emission at 1.01 keV is considered as convolution of Zn 2p3/2 and Zn 2p1/2 photoelectron energies. The occurrence of these peaks in the EDX endorses the existence of Zn and O atoms in the PSP prepared samples. HRTEM analysis has revealed NPs size modal range from 6.65-14.21 nm for the PSP synthesized samples which is in mutual agreement with the XRD data calculated values. More over the selected area diffraction images displaying the fact that only the diffraction planes of (101), (002) and (100) are responsible for the diffraction pattern belonging to Wurtzite ZnO. RS analysis has revealed that the un-doped ZnO and doped ZnO samples have characteristic Raman vibration modes at 325 cm-1, and 434 cm-1 belonging to Wurtzite ZnO structure. Moreover, the prominent peak at 434 cm-1 which is the characteristic peak of E2(2) (high) mode of the Wurtzite ZnO and the E2(2) (high) has been red shifted by 4 cm-1, as compared to that found in the bulk ZnO. Additionally, the effect of carbon doping through Raman spectroscopy peak shifts of the E2(2) (high) mode, A1(LO) mode and multi-phonon has also been considered and discussed in detail. UV-Vis diffuse reflectance spectroscopy has revealed a red shift of the absorption edge with increase in C doping. Finally, the effect of nano-crystallite size and gradual prominence of C into ZnO lattice due to increase in C doping concentration in the PSP prepared nanoparticles was meticulously elaborated through Raman Spectroscopy analysis.
- Full Text:
- Authors: Ntozakhe, Luyolo
- Date: 2017
- Subjects: Zinc oxide -- Synthesis Nanoparticles
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: http://hdl.handle.net/10353/5862 , vital:29408
- Description: In this work, the pneumatic spray pyrolysis was used to synthesize un-doped and carbon doped zinc oxide (ZnO) nanoparticles. The zinc acetate, tetrabutylammonium bromide and ethanol were used as starting materials for the desired ZnO nanoparticles and the prepared samples were annealed at 400 oC in the furnace. The as synthesized un-doped and carbon doped ZnO NPs were evaluated using X-ray diffraction (XRD), Scanning electron microscope (SEM), Energy dispersive x-ray spectroscopy (EDX), High-resolution transmission electron microscopy (HRTEM), Raman spectroscopy (RS) and Ultraviolet-visible spectroscopy (UV-Vis). XRD analysis of the synthesized NPs revealed peaks at 31.90°, 34.50°, 36.34°, 47.73°, 56.88°, 63.04°, 68.20°, and 77.33° belonging to the hexagonal Wurtzite ZnO crystal structure. The incorporation of C species into ZnO lattice was cross examined by monitoring the peak positions of the (100), (002) and (001) planes. These three main peaks of C-ZnO NPs show a peak shift to higher 2θ values which indicates substitutional carbon doping in ZnO NPs. SEM analysis has revealed that the as synthesized NPs have spherical shape and the morphology of the NPs change as the concentration of carbon increases. The EDX spectra of both un-doped and doped ZnO nanoparticles have revealed prominent peaks at 0.51 keV, 1.01 keV, 1.49 keV, 8.87 keV and 9.86 keV. Peaks at, X-ray energies of 0.51 keV and 1.01 keV respectively represent the emissions from the K-shell of oxygen and L-shell of zinc. The L-shell emission at 1.01 keV is considered as convolution of Zn 2p3/2 and Zn 2p1/2 photoelectron energies. The occurrence of these peaks in the EDX endorses the existence of Zn and O atoms in the PSP prepared samples. HRTEM analysis has revealed NPs size modal range from 6.65-14.21 nm for the PSP synthesized samples which is in mutual agreement with the XRD data calculated values. More over the selected area diffraction images displaying the fact that only the diffraction planes of (101), (002) and (100) are responsible for the diffraction pattern belonging to Wurtzite ZnO. RS analysis has revealed that the un-doped ZnO and doped ZnO samples have characteristic Raman vibration modes at 325 cm-1, and 434 cm-1 belonging to Wurtzite ZnO structure. Moreover, the prominent peak at 434 cm-1 which is the characteristic peak of E2(2) (high) mode of the Wurtzite ZnO and the E2(2) (high) has been red shifted by 4 cm-1, as compared to that found in the bulk ZnO. Additionally, the effect of carbon doping through Raman spectroscopy peak shifts of the E2(2) (high) mode, A1(LO) mode and multi-phonon has also been considered and discussed in detail. UV-Vis diffuse reflectance spectroscopy has revealed a red shift of the absorption edge with increase in C doping. Finally, the effect of nano-crystallite size and gradual prominence of C into ZnO lattice due to increase in C doping concentration in the PSP prepared nanoparticles was meticulously elaborated through Raman Spectroscopy analysis.
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Template-assisted sol-gel synthesis of carbon doped titanium dioxide nanotubes and their characterization
- Authors: Takata, Nwabisa
- Date: 2017
- Subjects: Nanotechnology Titanium dioxide Nanostructures
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: http://hdl.handle.net/10353/13194 , vital:39473
- Description: This study reveals the effects of doping on the morphological, structural and optical properties of titanium dioxide (TiO2) nanotubes (TNTs), synthesized by sol-gel template-assisted sol-gel technique. The nanotubes (TNTs) were prepared in anodic alumina membranes (AAM) with a pore diameter range of 110-210 nm by using titanium tetra butoxide as a sol-gel precursor and oxalic acid dihydrate as a dopant source. The synthesized nanotubes were evaluated using scanning electron microscope (SEM), energy dispersive spectroscopy (EDX), fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), confocal Raman spectroscopy (CRS) and photoluminescence spectroscopy (PL). SEM analysis has revealed the presence of closely-packed TNTs, with a modal external tube diameters of 150, 170, 210,190 and 210 nm for the un-doped TNTs, 9 mM carbon doped-TNTs (C-TNTs), 27 mM C-TNTs, 45 mM C-TNTs and 75 mM C-TNTs respectively. The diameters are consistent with the AAM diameter range. EDX spectra revealed the presence of Ti peaks at 0.45 and 4.9 keV corresponding to Kα1 and Kβ1 emission lines respectively. Oxygen exhibits a signal at 0.5 keV corresponding to Kα1 emission line. The occurrence of these peaks in the EDX spectra endorses the existence of Ti and O atoms in the prepared titanium dioxide nanotubes. FTIR spectroscopy has revealed the presence of vibration modes at 580-660 cm-1 indicating the presence of Ti-O bonds and additional vibration modes at 2324 cm-1 resulting from C-O stretching in the C-TNTs. The XRD analysis has revealed the presence of a mixed anatase-brookite phase with diffraction peaks at 2θ angles of 25.49⁰, 38.11⁰, 40.60º, 48.14⁰, 54.58⁰, 63.00⁰, 70.11⁰ and 75.66⁰. Additionally, XRD analysis has revealed elongation of lattice parameter “c” from 9.143 to 9.830 Å with carbon concentration increase. Lattice expansion indicates the possibility of carbon substituting oxygen sites. Raman large area scan has revealed the presence of rutile, brookite and anatase for the undoped samples. On doping the rutile phase of TiO2 has shown to be suppressed by the presence of carbon atoms such that the doped samples consist of brookite and anatase phases only. The Eg1 mode of anatase of the undoped TNTs at 153. 78 cm-1 was red shifted by Δ9.78 cm-1 relative to the bulk anatase TiO2. This was attributed to decrease in particle size, presence of brookite and phonon confinement. Upon doping, the 9 mM C-TNTs, 27 mM TNTs and 75 mM TNTs have shown a red shift of Δ0. 09 cm-1, Δ1. 39 cm-1 and 1.81 cm-1 respectively, suggesting the incorporation of carbon in the TiO2 matrix. CRS depth profiling in the XZ direction has also validated the presence of a mixed anatase-brookite phase at Raman active modes 153.19 cm-1, 208.87 cm-1, 404.55 cm-1, 523.26 cm-1 and 648.55 cm-1. Photoluminescence spectra of carbon doped TiO2 showed two emission peaks at 398 nm attributed to annihilation of excitons while the broad peak at 400-460 nm was attributed to the presence of oxygen vacancies. The peak intensity of the 45 mM C-TNTs has shown a lower PL intensity suggesting that efficiency of charge separation was higher and recombination rate was lower than other carbon containing samples.
- Full Text:
- Authors: Takata, Nwabisa
- Date: 2017
- Subjects: Nanotechnology Titanium dioxide Nanostructures
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: http://hdl.handle.net/10353/13194 , vital:39473
- Description: This study reveals the effects of doping on the morphological, structural and optical properties of titanium dioxide (TiO2) nanotubes (TNTs), synthesized by sol-gel template-assisted sol-gel technique. The nanotubes (TNTs) were prepared in anodic alumina membranes (AAM) with a pore diameter range of 110-210 nm by using titanium tetra butoxide as a sol-gel precursor and oxalic acid dihydrate as a dopant source. The synthesized nanotubes were evaluated using scanning electron microscope (SEM), energy dispersive spectroscopy (EDX), fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), confocal Raman spectroscopy (CRS) and photoluminescence spectroscopy (PL). SEM analysis has revealed the presence of closely-packed TNTs, with a modal external tube diameters of 150, 170, 210,190 and 210 nm for the un-doped TNTs, 9 mM carbon doped-TNTs (C-TNTs), 27 mM C-TNTs, 45 mM C-TNTs and 75 mM C-TNTs respectively. The diameters are consistent with the AAM diameter range. EDX spectra revealed the presence of Ti peaks at 0.45 and 4.9 keV corresponding to Kα1 and Kβ1 emission lines respectively. Oxygen exhibits a signal at 0.5 keV corresponding to Kα1 emission line. The occurrence of these peaks in the EDX spectra endorses the existence of Ti and O atoms in the prepared titanium dioxide nanotubes. FTIR spectroscopy has revealed the presence of vibration modes at 580-660 cm-1 indicating the presence of Ti-O bonds and additional vibration modes at 2324 cm-1 resulting from C-O stretching in the C-TNTs. The XRD analysis has revealed the presence of a mixed anatase-brookite phase with diffraction peaks at 2θ angles of 25.49⁰, 38.11⁰, 40.60º, 48.14⁰, 54.58⁰, 63.00⁰, 70.11⁰ and 75.66⁰. Additionally, XRD analysis has revealed elongation of lattice parameter “c” from 9.143 to 9.830 Å with carbon concentration increase. Lattice expansion indicates the possibility of carbon substituting oxygen sites. Raman large area scan has revealed the presence of rutile, brookite and anatase for the undoped samples. On doping the rutile phase of TiO2 has shown to be suppressed by the presence of carbon atoms such that the doped samples consist of brookite and anatase phases only. The Eg1 mode of anatase of the undoped TNTs at 153. 78 cm-1 was red shifted by Δ9.78 cm-1 relative to the bulk anatase TiO2. This was attributed to decrease in particle size, presence of brookite and phonon confinement. Upon doping, the 9 mM C-TNTs, 27 mM TNTs and 75 mM TNTs have shown a red shift of Δ0. 09 cm-1, Δ1. 39 cm-1 and 1.81 cm-1 respectively, suggesting the incorporation of carbon in the TiO2 matrix. CRS depth profiling in the XZ direction has also validated the presence of a mixed anatase-brookite phase at Raman active modes 153.19 cm-1, 208.87 cm-1, 404.55 cm-1, 523.26 cm-1 and 648.55 cm-1. Photoluminescence spectra of carbon doped TiO2 showed two emission peaks at 398 nm attributed to annihilation of excitons while the broad peak at 400-460 nm was attributed to the presence of oxygen vacancies. The peak intensity of the 45 mM C-TNTs has shown a lower PL intensity suggesting that efficiency of charge separation was higher and recombination rate was lower than other carbon containing samples.
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