近年來面臨石化燃料的儲量正在減少及其無限制的使用造成地球表面溫度和氣候的嚴峻變化，而水分解產生的氫的形式貯存太陽能是目前緩解全球變暖的理想方法之一。“金屬有機骨架”（MOF）的新興材料已開始被應用於光電催化劑，尤其是藉由光電化學途徑將水解離，它們極高的孔隙率以及多變的化學和結構可塑性，使其促進太陽光的吸收並提升光電化學離解水的潛在能力；利用控制MOF中所使用的不同鏈接結構或利用摻雜元素而調整能隙能量、有利於功能化各種基底材料、調節其耐腐蝕性與持久性，因此這類複合材料是催化、電催化或光電催化非常感興趣的電極材料之一；另一方面，例如以納米管或奈米纖維形式的奈米結構的二氧化鈦（二氧化鈦奈米微陣列（TNA））是非常適合構造用於在水介質中析出氧氣的光電化學之陽極材料，而這類材料的應用已經在文獻中進行了廣泛的討論，因此在我們的研究中，我們製造了由過渡金屬（Ni，Co，Fe）的MOF沉積在TNA（納米管或奈米纖維的微陣列結構）上製成的複合材料。我們使用了電沉積的電化學方法（循環伏安法），這使我們能夠將金屬氫氧化物以1.0 V的固定電勢均勻沉積在TNA上，然後通過與有機鏈結配體（1,3,5-苯三甲酸，BTC，1,4-苯二甲酸，BDC和咪唑，2MZ）進行水熱法轉化成為MOF結構。最後，我們所獲得的複合材料表現出卓越的光電催化活性和優異的光電化學耐久性，根據我們的結果與探討這些複合材料已成功地使用在光電催化電極並應用於氧釋放反應（OER）。

The continued use of fossil fuel reserves since the industrial revolution has led to their scarcity; it has also created deep climatic imbalances, measurable by the amplitude of the atmospheric temperature cycles. Storing incident solar energy in the form of hydrogen produced by photoelectrochemical dissociation of water suggests the possibility of combating global warming. The materials of the "Metal Organic Framework" (MOF) family are semiconductor-type photoelectrocatalysts, which are advantageous for this type of application. Their extremely high porosity and their great variability in chemical composition and structure allow their properties of absorption of solar radiation and of catalysis to be adjusted. By controlling the chemical composition and the doping of the linker used in the MOF, it is possible to adjust the energy of the band gap, to promote the functionalization on a wide variety of substrates or to adjust their corrosion resistance in various chemical environments. They are therefore materials of great interest for catalysis, electrocatalysis or photo-electro-catalysis. For its part, nanostructured TiO2, for example in the form of a micrometric thickness mat of nanotubes (TDNT) or nanorods (TDNR) forming TiO2 nano-arrays (TNA), is commonly used in the manufacture of photoanodes for the evolution of gaseous oxygen (OER) in an aqueous medium. During our thesis, we fabricated composite materials consisting of MOF of transition metals (Ni, Co, Fe) deposited on TNAs. For this, we used an electrochemical method of electrodeposition. This allowed us to deposit metal hydroxides on TNAs at fixed potential and then transform them by chemical reaction with organic ligands (BTC, BDC, and 2MZ) thermochemically. These photoelectrodes exhibit both a high level of photoelectrochemical performance and high stability against photo-corrosion. The reaction mechanisms were analyzed by photoelectrochemical impedance spectroscopy. The different steps have been identified and the values of the kinetic parameters have been determined over a wide range of potential. These composite materials have been used with success as the active phase of photoanodes for the OER. These photo-anodes have significant electrocatalytic activity and excellent photoelectrochemical durability.

ABSTRACT ......................................................................................................................... - I -
DECLARATION..........................................................................................................- III -
ACKNOWLEDGEMENTS .........................................................................................- IV -
TABLE OF CONTENTS.............................................................................................. - VI -
FIGURES AND TABLES INDEX .................................................................................. - IV -
ABBREVIATIONS....................................................................................................- XIII -
MOTIVATION ............................................................................................................- XIV
OBJECTIVES AND METHODOLOGY.....................................................................- XV1

INTRODUCTION ................................................................................................. - 1 -
1.1. WATER SPLITTING...........................................................................................- 1 -
Photo-electrochemical water splitting (PEC-WS) ................................................... - 5 -
1.2. METAL ORGANIC FRAMEWORK.......................................................................- 8 -
1.3. TITANIUM DIOXIDE NANOARRAY (TNAS)......................................................- 11 -
1.3.1 TiO2 nanotube arrays (TNTAs)..................................................................- 14 -
1.3.2 TiO2 nanorod arrays (TDNR) ....................................................................- 15 -
1.4. MOF/TNTA NANOCOMPOSITES....................................................................- 16 -

2. METHODOLOGY AND MATERIALS...............................................................- 20 -
2.1. CHEMICALS AND MATERIALS........................................................................- 20 -
2.2. SYNTHESIS OF VARIOUS MOFS......................................................................- 20 -
2.2.1 Cu-BTC-MOF...........................................................................................- 20 -
2.2.2 Fabrication of Cu-BTC-MOF-Ole and Boron doped Cu-BTC-MOF........- 21 -
2.2.3 Synthesis of Cu-Gly-MOF.........................................................................- 21 -
2.2.4 Synthesis of Ni-MOF.................................................................................- 21 -
2.3. SYNTHESIS OF TIO2 NANOARRAY..................................................................- 22 -
2.3.1 Production of TNTAs/Ti electrodes............................................................- 22 -
2.3.2 Production of TDNRs/FTO electrodes.......................................................- 23 -
2.4. SYNTHESIS OF MOF/TNA COMPOSITE.........................................................- 24 -
2.4.1 Formation of Ni-MOF on TDNRs/FTO ....................................................- 24 -
2.4.2 Formation of ZIF-67 MOF coating on TDNR ..........................................- 26 -
2.4.3 Formation of ZIF-67 MOF deposited on TDNR/FTO...............................- 27 -
2.4.4 Formation of FeNi-MOF on TNTA...........................................................- 28 -
2.5. ANALYTICAL TECHNIQUES FOR CHARACTERISTICS.....................................- 29 -
2.5.1 X-Ray Diffraction (XRD)...........................................................................- 29 -
2.5.2 Hard X-ray Absorption Spectroscopy.........................................................- 29 -
2.5.3 X-ray photoelectron spectroscopy (XPS)....................................................- 30 -
2.5.4 Brunauer−Emmett−Teller specific surface area analyzer (BET) ..............- 30 -
2.5.5 Scanning Electron Microscope (SEM)......................................................- 30 -
2.5.6 Transmission Electron Microscope (TEM)................................................- 31 -
2.5.7 Fourier transform infrared spectroscopy (FTIR) ......................................- 31 -
2.5.8 UV-Vis spectroscopy ..................................................................................- 31 -
2.5.9 Experiments for Electrochemical studies ..................................................- 31 -
2.5.10 Experiments for Photo-electrochemical measurements.........................- 32 -

3. FABRICATION OF MOFS BASED ON TRANSITION METALS WITH DIFFERENT LIGANDS FOR (PHOTO-) ELECTROCHEMICAL WATER SPLITTING ..................................................................................................................- 34 -
3.1 OBJECTIVE....................................................................................................- 34 -
3.2 INTRODUCTION .............................................................................................- 35 -
3.3 PHYSICAL CHARACTERIZATION....................................................................- 36 -
3.4 STRUCTURAL AND MORPHOLOGICAL CHARACTERIZATION .........................- 39 -
3.5 ELECTROCHEMICAL ANALYSIS .....................................................................- 43 -
3.6 CONCLUSIONS ...............................................................................................- 45 -

4. PHOTO-ELECTRO-OXIDATION OF WATER ON MATS OF TIO2 NANORODS
SURFACE MODIFIED BY NANOPARTICLES OF NI MOF....................................- 47 -
4.1 OBJECTIVE....................................................................................................- 47 -
4.2 INTRODUCTION .............................................................................................- 48 -
4.3 STRUCTURAL AND MORPHOLOGICAL CHARACTERIZATION .........................- 51 -
4.4 PHYSICAL CHARACTERIZATION....................................................................- 57 -
4.5 PEC ANALYSIS...............................................................................................- 62 -
4.6 CONCLUSION.................................................................................................- 66 -
4.7 SUPPORTING INFORMATION..........................................................................- 68 -

5. THE PERFORMANCE OF CALCINED RUTILE TIO2 NANORODS ARRAY
COATED BY A THIN LAYER NI-MOF AS PHOTOSENSITIZER APPLIED DURING
PEC WATER SPLITTING ...........................................................................................- 73 -
5.1 OBJECTIVE....................................................................................................- 73 -
5.2 INTRODUCTION .............................................................................................- 74 -
5.3 STRUCTURAL AND MORPHOLOGICAL CHARACTERIZATION .........................- 76 -
5.4 PHYSICAL CHARACTERIZATION....................................................................- 78 -
5.5 PEC ANALYSIS...............................................................................................- 81 -
5.6 CONCLUSION.................................................................................................- 85 -
6. FE/NI BIMETALLIC ORGANIC FRAMEWORK DEPOSITED ON TIO2
NANOTUBE ARRAY FOR ENHANCING HIGHER AND STABLE ACTIVITY OF
OXYGEN EVOLUTION REACTION.........................................................................- 87 -
6.1 OBJECTIVE....................................................................................................- 87 -
6.2 ARTICLE PUBLISHED IN NANOMATERIALS 2020, 10(9), 1688..............................- 87 -

CONCLUSION ...........................................................................................................- 101 -
REFERENCES............................................................................................................- 107 -
APPENDIX..................................................................................................................- 120 -
Electrochemically capacitive deionization of copper (II) using 3D hierarchically reduced
graphene oxide architectures ...................................................................................... -121 -
AUTOBIOGRAPHY ...................................................................................................... -132 -

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