用於電化學還原二氧化碳生成多碳產物的原子級電催化劑

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研究生：	KESEVEN LAKSHMANAN KESEVEN LAKSHMANAN
論文名稱：	用於電化學還原二氧化碳生成多碳產物的原子級電催化劑 Generating multi-carbon products from electrochemical reduction of CO2 by atomic electrocatalyst materials
指導教授：	蘇威年 Wei-Nien Su 黃炳照 Bing-Joe Hwang 蔡孟哲 Meng-Che Tsai
口試委員:	蘇威年 Wei-Nien Su 黃炳照 Bing-Joe Hwang 蔡孟哲 Meng-Che Tsai 潘俊仁 Chun-Jern Pan 林彥谷 Yan-Gu Lin 鄧熙聖 Hsisheng Teng
學位類別：	博士 Doctor
系所名稱：	應用科技學院 - 應用科技研究所 Graduate Institute of Applied Science and Technology
論文出版年：	2023
畢業學年度：	112
語文別：	英文
論文頁數：	161
中文關鍵詞：	原子級催化劑、多重活性位、CO2還原反應、C-C耦合、多碳產物
外文關鍵詞：	Atomic catalyst, multi-active sites, CO2 reduction reaction, C-C coupling, multi-carbon product
相關次數：	點閱：90 下載：1
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由於全球暖化和CO2排放引起的有害環境，迫切需要緩解這種情況，這是目前的當務之急。很明顯地，透過電化學CO2還原是一個有潛力的選擇，可以通過切斷碳循環來減緩CO2軌跡。此外，可以從CO2能量轉換中獲得CO和其他的碳氫產品。電催化劑材料在電化學能量轉換研究中發揮了至關重要的作用，能推動可持續的綠色能源生成和儲存，這可以應對不斷增長的全球能源需求。儘管貴金屬催化劑表現出色，但CO2還原反應(CO2RR)的動力學相當緩慢，因此開發先進的電催化劑材料仍有必要性。該材料應具有穩定的催化活性位點、動態的電子性能、操作耐久性和價格低廉，這對於可再生能源轉換技術來說是一個重要挑戰。
如今，單原子電催化劑材料因其高的表面能、獨特的電子性能、高表面積和最大的原子利用率而備受矚目。特別是，過渡金屬單原子催化劑成為決定性和有前途的電催化劑，它可以為反應中間體提供動態的電子平台，堅固的催化活性位點。在較高的施加電位下穩定，且成本效益高且豐富。加速基於過渡金屬的原子電催化劑對CO2RR的先進催化性能，探索反應機制、催化活性位點轉變以及其相關的基本性質仍然對設計獨特的原子電催化劑至關重要。然而，獲得具有合適配位環境、足夠金屬載荷和驗證催化活性位點的電子效應的獨特原子催化劑存在巨大的挑戰，這對於CO2RR是不可避免的。
因此，我們提出了過渡金屬單原子催化活性位點與共存於導電碳通道上的異質原子配位環境結合，用以改善CO2轉換的選擇性。這種設計將提高催化劑性能，實現更好的CO2轉換效率，並在催化活性反應中帶來基礎科學的清晰度。最終，這篇論文的目標是建立高效的電催化劑材料，並通過原位光譜電化學技術對催化活性位點演變、活性位點電子性質和電化學CO2還原過程中的產物反應途徑進行基本研究。
我們提出的第一個方法是解決Fe單原子催化劑(Fe SAC)對CO2電解的電催化活性和性能的問題。我們展示了一種獨特的單原子配位環境，其中Fe被三個氧原子包圍存在於HOOC-MWCNTs（Fe-n-f-MWCNTs）。顯著的是，Fe SAC是通過離子交換過程實現的，而不是高溫裂解熱處理，此合成方法非常簡便。Fe SAC的內部配位結構為CO2還原過程中的反應中間體提供了動態的催化活性位點，可以生成CO中間體。Fe原子在CO2電解過程中保持+3價態。Fe-(O)3活性位點降低了反應能障，加速電子轉移到COOH和*OCHO中間體，產生CO。MWCNTs上的COOH基團通過靜電力平衡Fe原子。最終，Fe-n-f-MWCNTs催化劑在-0.8 VRHE時對CO2轉換為C2產品的效能優越，達到65%的法拉第效率(FE)。氧協同配位結構對Fe SAC的協同效應產生影響，增強了反應途徑，實現了多電子轉移而不是雙電子轉移。產物的速率表明，Fe SA位點將大量的CO傳遞給HOOC-MWCNTs位點，形成C2產品。
第二種方法是應對二氧化碳還原反應開發中的挑戰，生產多碳產物，其中穩定的雙活性位點是不可避免的。我們引入了具有Ni和Cu單原子的酞氰分子(phthalocyanine)，共同作為雙活性催化位點。這種方法的目的是從第一種方法的模糊機制和性能結果中發現，儘管我們獲得了多碳產物作為主要產物，但第二個催化活性位點尚未被確定。因此，在這種方法中，我們提出了Ni/Cu雙催化活性位點，其中由Ni-Pc和Cu-Pc分子的物理混合過程衍生出了由Ni和Cu原子對組成的雙活性位點催化劑。顯著的是，Ni/Cu雙原子位點催化劑為協同作用的合理性質提供了近距離的兩原子對，觸發C-C偶聚反應，可以產生多碳產物進行CO2RR。Ni/Cu PASC催化CO2RR生成乙醇產物的電化學性能達到了55％的FE，而單獨的Ni-Pc和Cu-Pc僅生成單碳產物。值得注意的是，原位光譜電化學研究顯示，Ni/Cu雙活性位點催化劑的近距離原子對提供了穩定的活性位點，並在CO2RR下具有平衡的電子性質。
因此，穩定的Ni活性位點促使CO的一致生成，CO的遷移經歷了在Cu位點上形成的CO2中間體的C-C偶聚反應。最終，Ni/Cu雙活性位點催化活性的近距離對表明，兩個Ni和Cu單原子活性位點的和諧趨向於有效的CO2RR產生多碳產物。由於我們在第二種方法中探索的Ni/Cu近距離原子催化劑具有有限的電流密度，影響了多碳產物的產量，這激發了我們開發一種雙金屬單原子集成導電碳支撐催化劑的靈感。因此，第三種方法的目標是建立具有高電流密度的相容異質雙金屬單原子電催化劑。我們合成了Ni和Fe共存的雙金屬單原子峰值催化活性位點，與2D碳通道相關聯。

Owing to the global warming and noxious ambient caused by CO2 emission need to be alleviate and it is need of the moment. Significantly, the electrochemical CO2 reduction is the impressive choice that pull two weeds with one yank that can mitigate the CO2 trace via cut-off the carbon-cycles. In addition, intermittent feedstock of CO and such a high energy density chemicals of multi-carbon products can acquired from CO2 energy conversion. Electrocatalyst materials have been played pivotal role on electrochemical energy conversion research could advance the sustainable green energy generation and storage that can have challenge the thriving global energy demand. Even though, noble metal catalysts are performed, sluggish kinetics of the CO2 reduction reaction insist to develop an advanced electrocatalyst materials which is should have consists the stable catalytically active sites, dynamic electronic property, operationally durable and inexpensive materials are the considerable threat to the renewable energy conversion technologies perform in fuel cells.
Nowadays, single-atom electrocatalyst materials are rising star in the electrochemical energy conversion because of their tremendous surface energy, unique electronic property, high surface area, and maximum atom utilization. Especially, transition metal single-atom catalyst becomes decisive and promising electrocatalyst, which can render dynamic electronic platform to the intermediates accessibility, robust catalytic active sites, stable at higher applied potential, low-cost effectiveness and abundance. Accelerate the transition metal based atomic electrocatalyst for advanced catalytic performance toward CO2RR, it is inevitable to explore the reaction mechanism, catalytic active site transformation, and its related fundamental properties are remains of great importance to design unique atomic electrocatalyst. However, there is a huge quest to acquire the distinct atomic catalyst with suitable coordination environment, sufficient metal loading, and validate the electronic effect of catalytic active site is an inevitable for CO2RR.
Accordingly, we propose transition metals single-atom catalytic active sites hooked with hetero atom coordination environment co-existed on conductive carbon channel, deemed as leading candidate for the CO2 energy conversion. This design will advance the catalyst performance to reach the better efficiency towards CO2 conversion and also bring the clarity in fundamental science for the catalytic activity against CO2 reduction reaction. Eventually, this dissertation aim is to establish the productive electrocatalyst materials and its fundamental investigations of catalytic active site evolution, active site electronic property and product reaction pathway during the electrochemical CO2 reduction using in-situ spectro-electrochemical techniques. Thus, we have presented the consecutive approaches that encounter the challenges and establish the constructive solution for single-atom electrocatalyst against CO2 energy conversion.
Therefore, approach one addressing the electrocatalytical activity and performance of Fe SAC for CO2 electrolysis. We demonstrate a unique single-atom coordination environment that Fe has been surrounded by three oxygen atoms were exist on HOOC-MWCNTs (Fe-n-f-MWCNTs). Significantly, Fe SAC was achieved by ion exchange process instead of conventional high-temperature treatment, synthesis method was an effortless. The Fe SACs insight coordination structure renders dynamic catalytically active sites to the reaction intermediates during CO2 reduction, which could generate *CO intermediates. Fe atom maintain +3 valance state during CO2 electrolysis. The Fe-(O)3 active site decrease the energy barrier that accelerate the electrons to *COOH and *OCHO intermediates, producing CO. The COOH group on MWCNTs balance the Fe atom by electrostatic force. Eventually, the Fe-n-f-CNTs catalyst shows superior performance towards the CO2 conversion into C2 products record 65% FE at -0.8 VRHE. The presence of oxygen coordination configuration provokes the synergetic effect on Fe SA and enhances the reaction pathway toward multi-electron transfer instead of two-electron transfer. The rate of the product suggest that the Fe SA site deliver an enormous CO to the HOOC-MWCNTs site for C2 product formation.
Consecutively, second approach is addressing the challenges in the development of CO2 reduction reaction to produce multi-carbon product in which stable dual active sites are inevitable, we introduced Ni and Cu single-atom function together as dual active catalytic sites. Moreover, aim of this approach was discover from the ambiguous mechanism of first approach and its performance outcomes, in which, though we get multi-carbon product as a primary product, second catalytic active site have not been identified. Accordingly, in this approach we proposed Ni/Cu dual catalytic active site, where dual active site catalyst consisting Ni and Cu atomic pair was derived via physical mixing process of Ni-Pc and Cu-Pc commercial single-atom molecules. Significantly, Ni/Cu dual atom site catalysts render proximal two atom pair for the rational nature of synergetic action that trigger the C-C coupling reaction could produce multi-carbon products toward CO2RR. The electrochemical performance of Ni/Cu PASC catalyzed the multi-carbon product of ethanol with FE 0f 55%, whereas Ni-Pc and Cu-Pc has been recorded only single-carbon products. Notably, In-situ spectro-electrochemical studies have revealed that proximal atomic pairs of Ni/Cu dual active sites catalyst render stable active sites along with balanced electronic property under CO2RR.
Consequently, the consistent production of CO has facilitated by stable Ni active sites, migration of CO underwent C-C coupling with CO2 intermediates formed on the Cu sites. Eventually, the proximal pair of Ni/Cu dual active site catalytic activity concludes that two Ni and Cu single atom active sites harmonious tends sanctioned multi-carbon product toward effective CO2RR. As we explored the Ni/Cu proximal atom catalyst in approach two has limited current density which affects the volume of the multi-carbon production, it inspired us to develop a dual-metal single atom integrated conductive carbon support catalyst. Consequently, third approach aim is to establish the compatible heterogeneous dual-metal single-atom electrocatalyst with high current density. Thus, we synthesis Ni and Fe co-existing as dual-metal single-atom insight catalytic active site associated with 2D carbon channel.

中文摘要  i
Abstract  iv
Acknowledgment	viii
Table of contents  x
List of figures  xiii
List of units and abbreviations  xxv
Chapter 1: Introduction  1
1 CO2RR is the need of the hour  1
1.1	Promising technique of electrochemical CO2 conversion  2
1.2	Storage of high density intermittent renewable electricity  3
1.3	Rising star of single-atom catalyst  4
1.4	Significant of dual-active dual-metal atom catalyst  5
1.5	Multi-carbon product formation mechanism  6
2 Challenges and barrier in the single & dual-atom catalyst to produce multi-carbon products  7
2.1	Synthesis of single and dual-atom catalyst  7
2.2	Active sites stability  8
2.3	Active site mechanism	9
2.4	Mass transfer limitations  10
2.5	Flow cell application  12
3	Motivation  14
4	Objectives  16
Chapter 2: Literature Review: State of the art of atomic electrocatalysts toward CO2 reduction reaction  17
1 Synthesis of atomic catalyst  19
1.1	Wet chemical process  19
1.2	Impregnation method  19
1.3	Co-precipitation  21
1.4	Galvanic replacement  22
1.5	Coordination strategy  23
1.6	Atomic layer deposition  24
1.7	Pyrolysis  25
1.8	Spatial confinement strategy  26
1.9	Other synthetic approaches  27
2 Significant catalysts performance toward CO2RR  28
3	CO2RR active site Mechanism  34
4	Investigating CO2 reduction reaction mechanism toward multi-carbon formation  41
5	Generating value-added chemicals by CO2RR using MEA flow cell  45
6	Crucial approaches to advancing the catalyst performance for multi-carbon products  52
6.1	Synthesis single & multi-catalytic active site catalyst material  53
6.2	Tuning electronic properties of the metal active site  54
6.3	Structural morphology of the catalyst material  56
6.4	Tandem effect between metal active sites  58
6.5	MEA Flow cells  59
Chapter 3: 	Experimental section and characterization  61
1	Chemicals and reagents 61
2	Experimental methods  62
2.1	Synthesis of functionalized MWCNTs  62
2.2	Preparation of Nafion coated on f-MWCNTs and MWCNTs  62
2.3	Synthesis of Fe single-atom on n-F-MWCNTs and n-MWCNTs  63
2.4	Preparation of proximal Ni and Cu dual-active sites catalyst (Ni/Cu-PASC)  63
2.5	Synthesis of multi-atom on carbon-based catalyst materials  63
3	Materials characterization techniques  64
3.1	Physical characterization techniques  64
3.2	Electrochemical measurements and preparation of working electrode  65
3.3 In-situ X-ray characterization techniques  68
3.4 In-situ Attenuated total reflectance-Fourier-transform infrared (ATR-FTIR) spectroscopy  70
3.4	Density Functional Theory calculation detail  72
Chapter 4: 	Oxygen coordinated configuration of Fe singe-atom catalyst toward CO2RR into multi-carbon products  77
1 Scope of the study  77
2   Results and discussion  78
2.1	Fe SAC characterization for morphology  78
2.2	Fe single-atom performance toward CO2RR  85
2.3	In-sight Fe single-atom mechanistic analysis during CO2RR  89
2.4	Discussion of reaction mechanism toward CO2RR  99
3	Summary  102
Chapter 5: 	Generating multi-carbon products by electrochemical CO2 reduction via catalytically harmonious Ni/Cu dual active sites	103
1	Scope of the study  103
2 Results and discussions  104
2.1 Material characterizations  104
2.2 Ni/Cu-PASC’s electrochemical performance of CO2RR  108
2.3 Mechanistic of harmonious Ni/Cu dual-active site under CO2RR  115
2.4 CO2 intermediates C-C coupling mechanism  118
3 Summary  127
Chapter 6:	Generating high-value multi-carbon chemicals from CO2RR by multi-metal single-atom catalyst  129
1 Scope of the study  129
2 Results and Discussions  130
2.1 Material characterizations  130
2.2 Electrochemical performance of the SAC  135
3 Summary  138
Chapter 7: Conclusions and future perspectives  139
1	Conclusions  139
2 Future perspective  142
        Reference  144
List of publication 164
Conference presentation  165
                                

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