用於高效制氫的碳量子點支撐 CdS 光催化劑的形態誘導缺陷和晶體工程

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研究生：	比沙爾納哈克 Nahak, Bishal Kumar
論文名稱：	用於高效制氫的碳量子點支撐 CdS 光催化劑的形態誘導缺陷和晶體工程 Morphology-Induced Defects and Crystal Engineering of Carbon Quantum Dot-Supported CdS Photocatalysts for Efficient Hydrogen Production
指導教授：	曾繁根 Tseng, Fan-Gang
口試委員:	胡哲嘉 Hu, Chechia 陳燦耀 Chen, Tsan-Yao
學位類別：	碩士 Master
系所名稱：	原子科學院 - 工程與系統科學系 Department of Engineering and System Science
論文出版年：	2024
畢業學年度：	112
語文別：	英文
論文頁數：	119
中文關鍵詞：	硫化鎘、硫化鎘、硫空位、方面工程、光催化、氫氣
外文關鍵詞：	Cadmium Sulphide, Cadmium Sulphide, Sulphur Vacancy, Facet Engineering, Photocatalysis, Hydrogen generation
相關次數：	點閱：46 下載：0
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光致發光碳量子點（CQD）由於其優異的光學性質、強的限域效應和良好的導電性而引起了人們的廣泛關注。然而，CQD的可持續合成及其在水分解中的應用尚未得到很好的探索。在此，我們從葡萄糖合成了CQD和氮摻雜CQD，並透過水熱法將它們修飾到CdS奈米球上。使用各種光譜、顯微鏡和電化學技術對合成的光催化劑進行了徹底的表徵。據觀察，CQD 中氮的存在會導致活性位點阻塞，從而減少表面積。所開發的 CQD 負載 CdS 奈米球顯示光催化羅丹明 B 染料在 60 分鐘內降解 97%，並在 10 小時產生 80,450 μmolg-1 的氫氣。發現CQD的最佳負載量為3mL，進一步增加CQD的量會阻礙光與光催化劑的相互作用。
為了進一步提高產氫率，CdS 奈米花具有一種新穎的尺寸依賴性光穩定性，及其對硫空位和晶面的影響。為了進一步增強光催化性能，我們在 CdS 奈米結構上引入了CQD。所得複合材料表現出令人印象深刻的可見光響應氫生成速率，高達 120748 µmolg-1。這歸因於暴露的 CdS (002) 晶面和增加的硫空位有助於在延長的 30 小時內實現更好的電荷分離和更高的穩定性，這可以從 PL 曲線的壽命延長得到證明。所開發的光催化劑的可持續性透過綠豆植物生長進行了測試，證實了其環境友善性。

Photoluminescent carbon quantum dots (CQD) have drawn intense attention due to its excellent optical properties, strong confinement effect, and good electrical conductivity. However, sustainable synthesis of CQD and its application in water splitting has not been well explored. Herein, we synthesized CQD, and nitrogen doped CQD from glucose and decorated them onto CdS nanospheres via hydrothermal method. The synthesized photocatalysts were thoroughly characterized using various spectroscopic, microscopic, and electrochemical techniques. It was observed the presence of nitrogen at CQD causes blocking of active sites that reduces the surface area. The developed CQD loaded CdS nanospheres showed a photocatalytic Rhodamine B dye degradation of 97% in 60 min and hydrogen generation of 80,450 μmolg-1 in 10 hr. The optimal amount of CQD loading was found to be 3mL, further increasing the CQD amount hinders the light interaction with photocatalyst.
Further to enhance the hydrogen generation yield, a novel size dependent photostability of CdS nanoflowers has been reported, along its effect on sulphur vacancies and crystal facet. To further augment the photocatalytic performance, we introduce CQDs on CdS nanostructures. The resulting composite exhibited an impressive visible-light-responsive hydrogen generation rate of 120748 µmolg-1. This attributed to exposed CdS (002) crystal facet with increased sulphur vacancy helped in attaining better charge separation and increased stability over an extended 30-hour period, which can be evidenced from increased lifetime from PL curves. The sustainability of developed photocatalyst was tested via Vigna Radiata plant growth, that confirms its environmental friendliness.

Table of Contents
抽象的…………………………………………..……………………………………………..ii
Abstract…………………………………………..…………………………………………..iii
Acknowledgement…………………………………………..……………………………….iv
Abbreviations…….……………..…………………………..………………………………...v
List of Contents…...……………..…………………………..……………………………....vii
List of Figures…….……………..…………………………..………………………………xii
List of Tables……..………………………...………………..……………………………..xvii
Chapter 1: Visible Light Responsive Photocatalysis
1.    Introduction
1.1.    Rising CO2 Emissions………………………………………………..…………….1
1.2.    CO2 capture, Reuse and Recycle………………………………………………..….2
1.3.    Future Fuel- Hydrogen…………………………………………..…………………2
1.3.1.    Grey, Blue, Green Hydrogen………………………………………………......3
1.4.    Challenges and Implications involved in Hydrogen Economy…………………….3
1.5.    Water Pollution…………………………………….………….…………………...4
1.6.    Advanced Oxidation Process for wastewater treatment……………………..…..…4
2.    Solar Light driven Photocatalytic Systems…………………………………………….5
2.1.    Basic Mechanism behind photocatalysis………….……………………………….6
2.2.    Using Oxygenates for H2 production: Sacrificial agents……………………..…….8
2.2.1.    Sacrificial Reagent: Methanol……………………………………...………….9
Chapter 2: Carbon based non-noble metal co-catalyst
3.    Quantum Dots…………………………………………………………….…………..10
3.1.    Photoluminescence property of Carbon Quantum Dots……………………..……10
3.1.1.    Quantum confinement effect ……………………………………………..…..10
3.1.2.    Surface State Emissions……………………………………………………....11
3.1.3.    Molecular State Emissions…………………………………………………....11
3.2.    Synthesis of Carbon Quantum Dots………………………………………….…...12
3.2.1.    Top to Down approach……………………………………………………..…12
3.2.2.    Bottom Up approach….………………………………………………….…...12
3.2.2.1.    Hydrothermal ……...…………………………………………………………13
4.    Photocatalytic action of Carbon Quantum Dots……………………………………....15
4.1.    Carbon Quantum Dots as an individual photocatalyst ………………….………..15
4.2.    Photosensitization……………………………………………………………..….16
4.3.    Electron Mediators ………….……………………………………………………16
4.4.    Up conversion Photoluminescence………………………………………..……...17
4.5.    Modifications of Carbon Quantum Dots …………...…………………………….18
4.5.1.    In terms of Size…………………………………………………………..…...18
4.5.2.    Surface Functionalization…………………………………………………….19
4.5.3.    Elemental doping………………………………………………………..........19
Chapter 3: Cadmium Sulphide: Synthesis routes and tailoring its properties
5.    Why Cadmium Sulphide?…………………………………………..………………...21
5.1.    Crystal Structure, Optical properties, and Phase Transitions………………...…...21
5.2.    Synthesis strategies for CdS……………………………………………………....22
5.2.1.    Hydrothermal synthesis method ..………………………………………….....22
5.2.2.    Solvothermal Synthetic Methods…………………………………………..…22
5.2.3.    Template Methods and Template Free Methods……………………………...23
5.2.4.    Chemical Bath deposition…………………………………………………….23
5.3.    Drawbacks of CdS………………………………………………………..………24
6.    Enhancement of CdS based photocatalytic systems………………………..…..……..25
6.1.    Morphology dependent visible light photocatalysis …………………………..….25
6.2.    Sulphur vacancy………………………………………………………………….27
6.3.    Crystal Engineering………………………………………………………...…….29
6.4.    Use of electron rich co-catalyst……………………………………..…………….32
Chapter 4: Synthesis of Carbon Quantum Dots and its Properties
7.    Carbon quantum Dots……………………………………………………....………...34
7.1.    Experimentation details…………..………………………………………………34
7.1.1.    Characterization details……………………………………………………....34
7.1.2.    Materials Required…………………………………………………………...35
7.1.3.    Synthesis of Carbon Quantum Dots………………………………………..…35
7.2.    Results and Discussion…………………………………………………………...35
7.2.1.    X-Ray Diffraction………………………………………………………….....35
7.2.2.    Morphology Study-Transmission Electron Microscopy……………………...36
7.2.3.    Optical Properties…………………………………………………………….37
7.2.4.    Fourier Transform Infrared Spectroscopy…………………………………….39
Chapter 5 Synthesis of CQDs loaded CdS nanospheres
8.    Introduction ……………………………………………………………………...…..40
8.1.    Experimental details……………………………………………………………...41
8.1.1.    Materials Required………………………………………………………..….41
8.1.2.    CdS nanospheres……………………………………………………………...41
8.1.3.    Photocatalytic Experiment…………………………………………………....43
8.1.3.1.    Hydrogen generation…………………………………………………………43
8.1.3.2.    Dye degradation………………………………………………………………43
8.1.4.    Photocatalyst sustainability test…………………………………………..…..44
8.2.    Results and Discussion…………………………………………………………...45
8.2.1.    Morphological Properties: Scanning Electron Microscope and Transmission Electron Microscope……………………………………………………….....45
8.2.2.    X-Ray Diffraction…………………………………………………………...47
8.2.3.    Optical Properties………………………………………………………….....51
8.2.3.1.    Absorbance Spectroscopy………………………………………………….....51
8.2.3.2.    Photoluminescence……………………………………………………..…….53
8.2.4.    Fourier Transform Infrared Spectroscopy………………………………..…...55
8.2.5.    BET Surface area……………………………………………………………..56
8.2.6.    X-Ray Photoelectron Spectroscopy……………………………………..……57
8.3.    Photocatalytic Performance………………………………………………………61
8.3.1.    Rhodamine B dye degradation……………..……………………………..61
8.3.2.    Hydrogen Generation …………………………………………………….65
8.3.3.    Proposed Mechanism……………………………………………………..70
Chapter 6: Tailoring properties: Effects of morphology variation and crystal defects
9.    Introduction………………………….……………………………………………….73
9.1.    Experimental Details……………………………………………………………..74
9.1.1.    Materials Required……………………………………………………..…….74
9.1.2.    Synthesis of Bare CdS Nanorods………………………………………..……74
9.1.3.    Synthesis of CdS Nanoflowers…………………………………………..…...74
9.1.4.    Photocatalytic Experiment………………………………………………..…..75
9.2.    Results and Discussion…………………………………………………………...75
9.2.1.    Growth Mechanism…………………………………………………………..75
9.2.2.    Morphological analysis of photocatalyst…………………………………..…78
9.2.3.    Structural and Elemental analysis of Photocatalyst…………………………...80
9.2.3.1.    X-Ray Diffraction Analysis…………………………………………………..80
9.2.3.2.    Raman Spectroscopy…………………………………………………………83
9.2.3.3.    Fourier Transform Infrared Spectroscopy…………………………………….83
9.2.3.4.    BET surface and Pore size distribution……………………………………….84
9.2.3.5.    X-Ray Photoelectron Spectroscopy…………………………………………..86
9.2.4.    Spectroscopy analysis of Photocatalyst……………………………..………..88
9.2.4.1.    Band Structure Study…………………………………………………………88
9.2.4.2.    Photoluminescence Spectroscopy…………………………………………….90
9.2.5.    Electrochemical and surface defects analysis of photocatalyst………….........90
9.2.5.1.    Time Resolved Photoluminescence Decay Spectroscopy…………………….90
9.2.5.2.    Electro Impedance Spectroscopy…………………………….……………….91
9.2.5.3.    Transient Photocurrent Response…………………………………………….92
9.2.5.4.    Electron Spin Resonance Spectra…………………………………………….94
9.3.    Photocatalytic Performance……………………………………………………....95
9.3.1.    Rhodamine B dye degradation……………………………………..…..……..95
9.3.2.    Hydrogen generation…………………………………………………..……..99
9.3.3.    Proposed Mechanism……………………………………………………..…102
Conclusion……………………………………………………………………………….....105
References………………………………………………………………………..………...106


List of Figures
Chapter 1: Visible Light Responsive Photocatalysis
Fig 1.1 shows type of Hydrogen generation and the amount of CO2 liberated from it……….....2
Fig 1.2 shows the different Advanced Oxidation Process used for water sterilization…….…...4
Fig 1.3 shows basic mechanism involved in photocatalysis…………………..………………..6
Fig 1.4 shows band position of semiconductors in relation with the redox potentials of Water splitting. The position of the CB and VB edges are presented relative to the NHE at pH 0…......8
Chapter 2: Carbon based non-noble metal co-catalyst
Fig 2.1 shows (a) absorbance spectra representing the size tunability of PbS QDs 3-10 nm. (b) Simplified Jablonski diagram for surface state mediated fluorescence………………….……11
Fig 2.2 shows different results for synthesis of CQDs………………………………………...12
Fig 2.3 shows (a) excited-state processes for doped C-dots excited at core state (at 320 nm) and surface state (at 420 nm). (b) Steady-state absorption (solid lines) and emission (dashed lines) spectra and c) time-resolved emission measurements of the doped C-dots…...………………15
Fig 2.4 shows (a) C-dots without any surface modification. (b) C-dots modified with electron donor groups and (c) C-dots modified with electron acceptors group. (d–f) Density functional theory calculations performed on (a–c), respectively, to calculate the energy levels as well as HOMO and LUMO of the molecules…………………………………………………………17
Chapter 3: Cadmium Sulphide: Synthesis routes and tailoring its properties
Fig 3.1 shows a brief description about CdS properties and its potential applications………...21
Fig 3.2 shows the various synthesis routes for CdS photocatalysts…………………...………22
Fig 3.3 shows the DOS confinement of nanoparticles for different dimensionality…………..27
Fig 3.4 shows the regulation of band structure through phase unction with bonding region…30
Fig 3.5 schematic of the effect of solvent and additive/impurity molecules or ions on the morphological control of crystal facets……………………………………………………….31
Chapter 4: Synthesis of Carbon Quantum Dots and its Properties
Fig 4.1 shows the X-ray diffraction pattern of synthesized CQD samples…………………….36
Fig 4.2 shows the TEM images of synthesized Carbon Quantum Dots (CQDs)………………37
Fig 4.3 shows the absorbance (a, b) and photoluminescence spectrum (c) of synthesized CQDs and N-CQDs samples…………………………………………………………….…………...38
Fig 4.4 shows FTIR spectrum of CQDs and N-CQDs samples…………………………….....39
Chapter 5 Synthesis of CQDs loaded CdS nanospheres
Fig 5.1 shows the synthesis procedure of CQD@CdS nanospheres…………………………..42
Fig 5.2 shows (a) SEM and TEM images of (b) CQD@CdS, (c) CQD. (d-g) Elemental mapping, EDAX of (h) CQD@CdS and (i) N-CQD@CdS.......................................................45
Fig 5.3 shows the (a) particle size distribution of CQDs, Elemental mapping of (b) N-CQD@CdS, SEM images of N-CQD@CdS and PVP@CdS....................................................46
Fig 5.4 shows (a) diffraction pattern for all CdS samples. (b) SAED pattern and (c) lattice fringes of the developed CQD@CdS confirms its mixed phase structure…………………….49
Fig 5.5 shows absorbance spectrum of (a) PVP@CdS, (b) CQD@CdS and N-CQD@CdS and bandgap analysis was done using Tauc plot for CQD@CdS and N-CQD@CdS samples and (d) Photoluminescence spectra for different CdS samples…………………………………..……52
Fig 23 shows the FTIR spectra for all CdS samples…………………………………………..55
Fig 5.7  shows (a-c) BET surface area and (d) average pore size distribution, total pore volumes for all CdS samples…………………………………………………………………………...57
Fig 25 shows XPS spectra of full survey scan from PVP@CdS, CQD@CdS and N-CQD@CdS samples……………………………………………………………………………………….59
Fig 5.9 shows the XPS spectra of PVP@CdS, CQD@CdS and N-CQD@CdS samples with their respective (a, d, g) Cd 3d, (b, e, h) S 2p and (c, f, i) C 1s elements and (j) ESR spectra of CQD@CdS and N-CQD@CdS samples……………………………..………………………60
Fig 5.10 shows Rhodamine B degradation absorbance spectrum by (a) N-CQD@CdS (b) CQD@CdS samples. (c) dye degradation efficiency and pseudo-second order kinetic plot (d) color change of dye in 60 min time period……………………………………………………64
Fig 5.11 shows (a) time dependent photocatalytic hydrogen generation, (b) average hydrogen generation rate in every hour by all CdS samples. The average hydrogen generation with (c) varying the (c) ratio of CQD and CdS and with (d) amount of CQD@CdS photocatalyst……67
Fig 5.12 shows the (a) time dependent hydrogen generation in seawater for 10 hrs time period, (b) average hydrogen generation by all CdS samples in seawater. (c) EIS spectroscopy and (d) mott-schottky pots for CQD@CdS and N-CQD@CdS samples. (e) shows the photo catalyst reusability and time dependent photocurrent for CQD@CdS samples……………………….68
Fig 5.13 shows (a) band positions of CQD@CdS and N-CQD@CdS photocatalyst. The photocatalytic hydrogen generation mechanism (b) for phase engineered, sulphur vacancy enriched and CQD loaded CdS nanostructures……………………………………………….71


Chapter 6: Tailoring properties: Effects of morphology variation and crystal defects
Fig 6.1 shows (a) synthesis procedure and growth mechanism of CdS nanorods and nanoflowers with varying solvothermal time. SEM images of (b) Bare CdS NRs, (c) CQD@CdS12NFs, (d) CQD@CdS24NFs. TEM images and d-spacing for (e, f) CQD@CdS12NFs and (g, h) CQD@CdS24NFs. Elemental mapping of (i-l) CQD@CdS12NFs....................................................................................................................77
Fig 6.2 shows TEM image confirming the presence of CQD in CQD@CdS12NFs (a) and individual CQD samples (b) ……………………………………………………...…………..78
Fig 6.3 shows the SEM elemental presence (a) of Cd, S, C, O in CQD@CdS24NFs sample, EDAX elemental mapping (b-e), EDAX spectrum of Bare CdS NRs (f), CQD@CdS12NFs (g) and CQD@CdS24NFs (h) …………………………………………………………………....79
Fig 6.4 shows diffraction pattern (a), Raman spectra (b), FTIR spectra (c), surface area for all CdS samples……………………………………………………………….............................81
Fig 6.5 shows XPS full survey scan (a), Cd 3d spectrum (b), C 1s spectrum (c) and S 2p spectrum (d) for all CdS samples……………………………………………………..………86
Fig 6.6 shows absorbance spectra (a), photoluminescence emission spectra (b), energy bandgap Tau-plot (c) and Mott-Schottky plot (d) for all CdS samples…………………………………88
Fig 6.7 shows Transient Responsive photoluminescence Decay spectra (a), electro impedance spectra (b), electron paramagnetic spectra (c) and transient photocurrent for all CdS samples.93
Fig 6.8 Nyquist equivalent circuit plot for EIS spectroscopy…………………...…………….93
Fig 6.9 shows Rhodamine B absorbance decay profile for (a) Bare CdS NRs, (b) CQD@CdS12NFs, (c) CQD@CdS24NFs.  Concentration (d) decay profile as a function of time and (e) linear fit obtained for pseudo-second order kinetic model and (f) real-time color change of dye for all CdS samples. Variation in (g, h) growth rate, (i) length of roots and shoots in Vigna Radiata for a period of 72h using different water samples…………………………..95
Fig 6.10 shows (a) time dependent photocatalytic H2 evolution, (b) stability test for H2 evolution, (c) average hydrogen production rates and (d) hydrogen production rate in absence of sacrificial reagents for all CdS samples……………………………………………….……99
Fig 6.11 shows H2 generation of CQD@CdS12NFs with varying amount of photocatalyst...100
Fig 6.12 shows change in morphology of all CdS based photocatalyst (a) before, (b) after 10 hours and (c) after 30 hours of hydrogen generation………………………………………...101
Fig 6.13 shows the band alignment positions of CdS nanoflowers and nanoclusters………..102
Fig 6.14 shows the (a) DFT calculated DOS band for Bare CdS and carbon loaded with Svacancy CdS in (002) facet orientation. (b) band structure positions of different CdS morphology photocatalysts. (c) possible mechanism for photocatalytic hydrogen generation…………....103








List of Tables
Chapter 1: Visible Light Responsive Photocatalysis
Table 1.1 shows the advantages and disadvantages of various synthesis methods……………14
Chapter 5 Synthesis of CQDs loaded CdS nanospheres
Table 5.1 shows the structural parameters crystallite size, average strain, and dislocation density of synthesized CdS samples…………………………………………………….….....50
Table 5.2 shows the Bandgap and Size of synthesized CdS samples……………………….…53
Table 5.3 shows Functional groups of PVP@CdS, CQD@CdS and N-CQD@CdS samples with respective to their wavenumber from FTIR spectroscopy………………………..……...55
Table 5.4 shows atomic percentage of Cadmium and Sulphur and their atomic ratio in all samples……………………………………………………………………..………………...61
Table 5.5 shows the band structure parameters such as Ef, Eg, ECB and EVB of CdS samples….70
Chapter 6: Tailoring properties: Effects of morphology variation and crystal defects
Table 6.1 shows the EDAX atomic % of Cd, S and intensity ratio for all CdS samples……….80
Table 6.2 shows intensity ratios for the planes (200) and (100), crystallite size, dislocation density and average strain for all CdS samples……………………………………………..…83
Table 6.3 shows the surface area, average pore width and pore volume for all CdS samples..85
Table 6.4 shows XPS atomic % of Cd, S, C and O for all CdS samples………………………87
Table 6.5 shows the energy bandgap, flat band potential, conduction band and valance band for all CdS samples………………………………………………………………………..….90
Table 6.6 shows kinetic analysis of emission decay for the CdS samples…………………….91
Table 6.7 shows the Nyquist plot fitting parameters for all CdS samples…………………….94
Table 6.8 Comparison of RhB dye degradation obtained in this study with literatures96…….98
Table 6.9 comparison of photocatalytic hydrogen generation obtained in this study with literatures……………………………………………………………………………………104


                                

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