Title of Thesis

Synthesis And Characterization Of Copper/mixed-Metal Copper Oxides From Single Source Precursors

Author(s)

MUHAMMAD SHAHID

Abstract
Several new monometallic, homobimetallic and heterobimetallic complexes such as [Ni(hfacac)2(dmaeH)] (1), [Cu(dmap)(OAc)(H2O)]2⋅H2O (2), [Cu2(OAc)3(dmap) (THF)]n (3), [Cu(dmae)(TFA)]4 (4), [Cu(deae)(TFA)]4 (5), [Cu4(OAc)6(bdmap)2 (H2O)2]⋅2H2O (6), [Cu6(bdmap)3(μ-O)2Cl6] (7), [Zn6(OAc)8(μ-O)2(dmae)4] (8), [Co(acac)Cu2(bdmap)2Cl3]⋅C7H8 (9), [Co(acac)Cu2(bdmap)2Cl3]⋅3CH2Cl2 (10), [Zn(TFA)3(μ-OH)Cu3(dmae)3Cl]∙THF (11), [Zn(TFA)4Cu3(dmae)4] (12), [Zn2(OAc)6 (μ-O)Cu4(dmae)4]⋅2H2O (13), [Zn2(OAc)6(μ-O)2Cu4(bdmap)2Cl2] (14), [Cd2(OAc)6(μ- O)Cu4(dmae)4]⋅H2O (15), [Ba2(dmae)4Cu4(OAc)6(OH)2] (16) and [Pb2(OAc)4(μ-O)3 Cu6(dmae)4Cl4]∙C7H8∙1.7H2O (17) were successfully synthesized and characterized by their melting point, elemental analysis, FT-IR, mass spectrometry, TGA and their molecular structures were determined by single crystal X-ray analysis. Thermogravimetric analyses prove that precursors undergo facile thermal decomposition at relatively low temperature to give copper/mixed-metal copper oxides. All the designed precursors except (1), (3) and (10), were used for the fabrication of thin films of copper/mixed-metal copper oxides by aerosol-assisted chemical vapour deposition. The phase crystallinity of deposited thin films was determined by XRD, while SEM and EDX were used for surface morphology and elemental composition.
The homometallic precursors (2), (4), (5), (6) and (7) have been found suitable for the deposition of Cu metal, while ZnO films were fabricated from precursor (8) under ordinary conditions of temperature and pressure, using nitrogen as carrier gas. The heterometallic precursors (9), (10) are promising for the deposition of Cu-CoO composite thin films, while (11), (12), (13), (14) for fabrication of Cu-ZnO and (15) for Cu-CdO composite thin films. Similarly, precursor (16) is suitable for CuO-Ba2Cu3O5+x and (17) for Cu-Pb2O3 ceramic thin films.
The powder XRD and EDX analysis revealed the formation of crystalline thin films by AACVD without any carboneous impurities and the SEM results demonstrated that the deposited films are crack free with particles having distinct and clear grain boundaries. These characteristics make them suitable for their possible technological applications. The thickness and voltage-current measurements of the films deposited from precursors (8) and (16) revealved their semiconducting nature, while the films fabricated from (11), (12) and (14) are ohmic conductors.

1

1 Material Science

2 Thin Film Technology

3 Characterization Techniques

1 General Considerations

2 Syntheses

3 X-ray Crystallography

4 Deposition of Thin Films

1 Structural Analysis of Homometallic Complexes

2 Structural Analyses of Heterobimetallic Complexes

3 Thermogravimetric Study and Characterization of Thin Films