Electrochemical Reduction of Co2

Electrochemical Reduction of Co2
اسم المؤلف
Muhammad Irfan Malik
التاريخ
30 نوفمبر 2020
المشاهدات
التقييم
(لا توجد تقييمات)
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رسالة ماجستير بعنوان
Electrochemical Reduction of Co2
By
Muhammad Irfan Malik
a Thesis Presented to the
38 Deanship of Graduate Studies
King Fahd University of Petroleum & Minerals I
Dhahran, Saudi Arabia
In Partial Fulfillment of the
Requirements for the Degree of
Master of Science
Chemical Engineering
Table of Contents
Acknowledgments V
Table of Contents . Vi
List of Tables Ix
List of Figures X
List of Abbreviations Xiii
Abstract Xiv
Xviملخص الرسالة
Chapter 1 Introduction . 1
Chapter 2 Literature Review . 6
2.1 CO2 reduction methods . 6
2.1.1 Hydrogenation of CO2/CO 6
2.1.2 Electrochemical CO2 reduction .10
2.1.3 Photochemical reduction of CO2: .19
2.2 A detailed review of electrochemical CO2 reduction . 22
2.3 Mechanism of electrochemical CO2 reduction to hydrocarbon and alcohols . 31
2.4 Objective . 41
CHAPTER 3 RESEARCH METHODOLOGY 43
3.1 Materials and Preparation 43
3.1.1 Impregnation of cupric oxides on carbon nanotubes 44
3.1.2 Impregnation of cuprous oxides on carbon nanotubes .45
3.2 Material Characterization . 45vii
3.2.1 Thermogravimetric Analysis (TGA) .46
3.2.2 Scanning Electron Microscopy (SEM) .46
3.2.3 X-ray diffractogram (XRD) 47
3.2.4 Transmission Electron Microscopy (TEM) 47
3.2.5 Raman Spectroscopy 48
3.3 Electrochemical Setup . 48
3.3.1 Working electrode Preparation 50
3.3.2 Design of electrochemical Cell .51
3.3.3 Nafion 117 Membrane .53
3.3.4 Cupric oxide and cuprous oxide based working electrodes .54
3.4 Electrochemical Test . 55
3.4.1 Linear sweep voltammetry .55
3.4.2 Choronoamperometry .56
Chapter 4 Results and Discussion 58
4.1 Physical Characterization 58
4.1.1 SEM and EDX analysis .58
4.1.2 Energy dispersive X-ray (EDX) analysis .65
4.1.3 X-ray diffraction Analysis (XRD Analysis) 69
4.1.4 Thermogravimetric analysis (TGA) .72
4.1.5 Raman Spectroscopy 73
4.1.6 N2 adsorption isotherms 75
4.1.7 Transmission electron microscopy (TEM) 76
4.2 Linear sweep voltammetry for carbon nanotubes loaded Cu2O based electrocatalyst 79
4.3 Linear sweep voltammetry for carbon nanotubes loaded CuO based electrocatalyst . 81
4.3.1 Comparative analysis of Linear Sweep Voltammetry results based on 30% Copper oxides
loading on CNT .82
4.4 Faradic Efficiency 83
4.4.1 Detailed analysis of Faradic Efficiency results .85
4.5 Chronoamperometry Analysis . 86
CHPTER 5 Density Functional Theory 88
5.1. Quantum Mechanical Modeling . 88
5.2. The Khon-Sham molecular orbital (MO) model 89
5.3. Simulation Method . 90viii
Chapter 6 Conclusion & Recommendations .93
6.1 Conclusion 93
6.2 Recommendations 94
References 95
Appendix 106
Internal standard method of calibration 106
Vitae . 108ix
LIST OF TABLES
Table 2-1: Periodic table of elements tested for CO2 reduction at -2.2 V vs SCE in .05M
Potassium bicarbonate solution KHCO3 at low temperature condition [44] 13
Table 2-2: Current efficiency for CO2 reduction products at -2.2V vs SCE in potassium
bicarbonate (.05M KHCO3)[44] . 15
Table 2-3: Summery of different electrocatalyst and their role on current density and
.faradic efficiency . 38
Table 5-1: Calculated Band gaps for Cu2O and Cu2O supported CNTs . 90x
LIST OF FIGURES
Figure 2-1: IR adsorption spectra of adsorb species methoxy and formats on catalyst
.surface of clean Cu(111) and ZnCu+(111) during formation of methanol by
hydrogenation at 343k and 1 atm[38] . 9
Figure 2-2: Development process of hole (h+) and e- upon UV irradiation by photo
.catalyst [51] 19
Figure 2-3: Time dependence effect on methanol formation for titanium and titanium
loaded Cu [57] . 21
Figure 2-4: Structure of Cu2O [66]. 29
Figure 3-1: Working electrode 49
Figure 3-2: Platinum counter electrode . 49
Figure 3-3: Reference Ag/AgCl electrode 50
Figure 3-4: Poly carbonate made electrochemical cell with two compartments separated
.by nafion membrane for electrochemical reduction of CO2 53
Figure 4-1: SEM image of 10% CuO supported CNT catalyst 59
Figure 4-2: SEM image of 20% CuO supported CNT catalyst 60
Figure 4-3: SEM image of 30% CuO supported CNT catalyst 60
Figure 4-4: SEM image of 40% CuO supported CNT catalyst 61
Figure 4-5: SEM image of 50% CuO supported CNT catalyst 61
Figure 4-6: SEM image of 10% Cu2O supported CNT catalyst . 63
Figure 4-7: SEM image of 20% Cu2O supported CNT catalyst . 63
Figure 4-8: SEM image of 30% Cu2O supported CNT catalyst . 64
Figure 4-9: SEM image of 40% Cu2O supported CNT catalyst . 64xi
Figure 4-10: SEM image of 50% Cu2O supported CNT catalyst . 65
Figure 4-11: EDX image of 10% Cu2O supported CNT catalyst . 66
Figure 4-12: EDX image of 40% Cu2O supported CNT catalyst . 67
Figure 4-13: EDX image of 20% CuO supported CNT catalyst 68
Figure 4-14: EDX image of 50% CuO supported CNT catalyst 69
Figure 4-15: XRD pattern for CuO supported CNT catalyst 71
Figure 4-16: XRD pattern for Cu2O supported CNT catalyst . 71
Figure 4-17: Thermogravimetric curves for Cu2O supported CNT catalysts . 73
Figure 4-18: Raman spectra of CuO supported CNT catalysts . 74
Figure 4-19: Raman spectra of Cu2O supported CNT catalysts . 75
Figure 4-20: Adsorption-desorption isotherm for CNT without loading . 76
Figure 4-21: TEM image of 10% CuO supported CNT catalyst 77
Figure 4-22: TEM image of 50% CuO supported CNT catalyst 77
Figure 4-23: TEM image of 10% Cu2O supported CNT catalyst . 78
Figure 4-24: TEM image of 50% Cu2O supported CNT catalyst . 78
Figure 4-25: LSV profiles for Cu2O supported CNT in CO2 saturated electrolyte 80
Figure 4-26: LSV profiles for CuO supported CNT in CO2 saturated electrolyte 82
Figure 4-27: LSV profiles for CNT loaded with 30% Cu2O and CuO in CO2 saturated
.electrolyte . 83
Figure 4-28: Faradic Efficiency of Methanol formation . 84
Figure 4-29: Current responses for Cu2O supported CNTS at constant potential in CO2
.saturated electrolyte . 87
Figure 5-1: Optmized structure of Cuprous oxide (Cu2O) P type semiconductor 91xii
Figure 5-2: Optimized structure of Cu2O supported carbon nanotube . 92xiii
LIST OF ABBREVIATIONS
CNTs : Carbon nanotubes
Pt : Platinum
Ag/AgCl : Silver/Silver Chloride
LSV : Linear Sweep Voltammetry
DFT : Density Functional Theory
SHE : Standard Hydrogen Electrode
XRD : X-ray-Diffraction
TEM : Transmission Electron Microscopy
EDX : Energy Dispersive X-ray
TGA : Thermo Gravimetric Analysis
SEM : Scanning Electron Microscopy
MWCNT : Multi walled Carbon Nanotubes
HER : Hydrogen Evolution Reaction
CuO : Cupric Oxide
Cu2O : Cuprous Oxide
ACF : Activated Carbon Fiber
SCE : Standard Calomel Electrode
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