I= SYNTHESES OF BIMETALLIC PRECURSORS FOR CERAMIC MATERIALS
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Title of Thesis
SYNTHESES OF BIMETALLIC PRECURSORS FOR CERAMIC MATERIALS

Author(s)
MAZHAR HAMID
Institute/University/Department Details
Department of Chemistry/ Quaid-i-Azam University Islamabad, Pakistan
Session
2008
Subject
Inorganic Chemistry
Number of Pages
191
Keywords (Extracted from title, table of contents and abstract of thesis)
ceramic materials, bimetallic complexes, trimetallic complexes, chemical vapor deposition, thin films, monometallic complex, homobimetallic complex, heterobimetallic complex, heterotrimetallic complex

Abstract
Several new single metal, bimetallic (homo and hetero) and trimetallic complexes such as [Zn(acac)2(dmae)] (1), [pd(acac)2) (2), [pdCl(dmae)dmaeH] (3), [Zn6(OAc)8(µ-OH)2-( dmae)2(dmaeH)2)(4),[Cu(dmae)Cl]4(5),[Cu3(acac)2(dmae)3Cl](6),[Co2(acac)2(µOH)2Cu4(dmae)4C14](7),[Ni2(acac)2-(µ-OH)2Cu4(dmae)4Cl4](8),[Co4(THF)4(TFAc)8Cu2(dmae)2)(9),[Zn7(OAc)1O(µ-OH)6Cus(dmae)4C14]2(C6H5-CH3) (10), [TlNi(acac)2(dmae)2 (11), [TlBa(acac)Ni2(acac)4(dmae)2 H20] (12) have been synthesized and characterized by their melting point, elemental analysis, FTIR, proton NMR, mass spectrometry, magnetometry, TGA and their molecular structures were determined by X-ray single crystal analysis. Thermogravimetric analysis prove that precursors undergo facile thermal decomposition at relatively low temperature (320-460°C) to give mixed metal oxides. The bimetallic and trimetallic complexes were used for the growth of thin films of monometallic, bimetallic and trimetallic oxides by aerosol assisted chemical vapor deposition. Thin films, thus grown were characterized by SEM for surface morphology, EDX for elemental composition and nature of crystalline product was determined by XRD.

The precursors have been found suitable for deposition of thin films under ordinary conditions of temperature and pressure; (4) for deposition of ZnO, (7) for CUo.30C02.704 and CuO, (8) for Nio.95CUo.O5O4 and CuO, (9) for CUo.75C02.2504 and CuO, (10) for CuO and ZnO, (11) for Tl203 and NiO, and (12) for Tl203, NiO and BaO.

Thin films were found to have no cracks, good adhesion and to be crystalline in nature without any carboneous impurities. Distinct crystallites have clear grain boundaries with particle sizes ranging from 0.55 to 2.9µm. These characteristics make them suitable for their possible technological applications.

Download Full Thesis
4702.02 KB
S. No. Chapter Title of the Chapters Page Size (KB)
1 1 Inorganic Chemistry Of Materials 1
962.72 KB
  1.1 Type Of Material 1
  1.2 Ceramic Material 2
  1.3 Mixed Metal Oxides 6
  1.4 Properties Of Ceramic Materials 7
  1.5 Synthesis Of Ceramic Materials 18
2 2 Chemical Vapor Deposition 29
244.52 KB
  2.1 CVD Equipment 30
  2.2 Types Of Chemical Vapor Deposition Technique 31
  2.3 Aerosol €“Assisted Chemical Vapor Deposition 31
  2.4 Type Of Reactions Taking Place During CVD Process 33
  2.5 Applications Of Chemical Vapor Deposition 35
  2.6 Chemical Vapor Deposition Precursors 35
3 3 Characterizing Techniques 56
2540.07 KB
  3.1 X-Ray Crystallography 56
  3.2 Nuclear Magnetic Resonance 58
  3.3 Mass Spectroscopy 58
  3.4 Ir Spectroscopy 58
  3.5 Elemental Analysis 60
  3.6 Thermo Gravimetric Analysis 60
  3.7 Film Adhesion Test 60
  3.8 Auger Electron Spectroscopy 61
  3.9 X-Ray Photoelectron Spectroscopy 62
  3.10 Scanning Electron Microscopy 63
  3.11 X-Ray Diffraction 64
4 4. Experimental
2540.07 KB
  4.1 General Considerations 66
  4.2 X-Ray Crystallography 68
  4.3 Deposition Of Thin Films 69
  4.4 Synthesis 72
5 5 Attempted Reactions 77
190.94 KB
  5.1 Reaction Of [ Cu( Dmae ) Ci ] 4 And [Ti( Dmae ) 4 ] 77
  5.2 Reaction Of [ Cu( Dmap ) Ci ]X And [Ti( Dmap ) 4 ] 78
  5.3 Reaction Of [ Cu( Dmae ) Cl ] 4 And [Zn( Acac ) 2 ] 78
  5.4 Reaction Of [ Cul ( Dmae )C] 4 And [ Cd ( Acac ) 2 ] 78
  5.5 Reaction Of [ Cu( Dmae ) Cl ] 4 And [ Zr ( Acac ) 3 ] 79
  5.6 Reaction Of [ Cu( Dmae ) Ci ] 4 And[ Ba ( Thd ) 2 ] 79
  5.7 Reaction Of [ Ba ( Dmae ) 2 ] And [Ni( Acac ) 2 ] 79
  5.8 Reaction Of [ Tl ( Acac )], [Co( Acac ) 2 ] And [ Dmaeh ] 79
  5.9 Reaction Of [ Tl ( Acac )], [Co( Acac ) 2 ] And [ Ba ( Dmae ) 2 ] 80
6 6 Results And Discussion
789.92 KB
  6.1 Structural Analysis Of Monometallic Complex 81
  6.2. Structural Analysis Of Homobimetallic Complex 94
  6.3. Structural Analysis Of Heterobimetallic Complex 107
  6.4. Structural Analysis Of Heterotrimetallic Complex 138
  6.5 . Products From Attempted Reaction 144
  6. 6 Thermogravimetric Study And Characterization Of Thin Films 153
7 7 Consclusions 178
789.92 KB
  7.1 References 180
  7.2 List Of Publications 191