鑑於電化學觸媒在綠色可持續能源生產、儲存和轉換中的核心作用，開發具高催化活性的先進奈米材料以滿足不斷增長的全球能源需求為重要研究領域。然而，開發用於析氧（OER）和氧還原反應（ORR），且具備操作穩定且廉價的雙功能觸媒材料是可再生能源存儲和轉換技術（例如金屬 - 空氣電池和燃料電池）中巨大挑戰之一。由於OER和ORR的反應動力學相當緩慢，即便使用貴金屬催化劑如鉑（用於ORR），氧化釕（用於OER）和氧化銥（用於OER）也是如此。因此，一個關鍵點在於開發具有出色催化活性，低成本和高耐久性的堅固觸媒材料，以同時用於難以進行的ORR/OER。
目前，過渡金屬氫氧化物/氧化物和鎳基層狀雙氫氧化物（LDHs）的電化學觸媒是鹼性電解質中有潛力的新型電極替代品，因為它們具有低成本，蘊藏量豐富，及催化OER / ORR的優秀能力和操作穩定性。在高pH的電解質下。為了加速鎳基層狀氫氧化物觸媒的開發，提高OER/ORR的催化活性，必須了解觸媒在鹼性OER和ORR操作過程中的反應機制，真實的活性位置和一些電位相關的表面性質，這些對於新型電化學觸媒的設計非常重要。
本論文旨在開發耐久、廉價及高效的雙功能電化學觸媒。在室溫鹼性條件下操作，利用臨場光譜電化學技術研究OER過程中的繼志，活性位點和表面性質。因此，開發了一類新的鎳基LDHs電催化劑（NiRu-LDHs和NiMn-LDHs奈米片），並與導電載體（銀奈米粒子（Ag奈米粒子）和銀奈米線（Ag NWs））結合，藉由修飾作用和核-殼結構之策略製備具有OER和ORR的雙功能電催化劑。這種方法對於下一代可逆氧電極的設計有很大益處，其涉及將較便宜的單功能OER和ORR電催化劑組合到一個混合系統中。
第一種方法（第4章）研究“銀奈米粒子修飾NiRu層狀雙氫氧化物奈米片進行氧氣析出和還原反應。這項工作的重點是新型電催化劑的開發;經由Ag NPs對NiRu-LDH的修飾作用，在鹼性下能有效催化OER和ORR且穩定，並且能區分與整體催化活性相關的位置活性(site activity)和活性位點分布(site population)。Ag NP/NiRu-LDHs上較高的ORR活性主要歸因於Ag位點活性的增加和更多的Ag活性位置數目。增加的Ag位點活性廣泛地來自Ag位點上發生的電荷極化，這弱化Ag位點上的OH吸附，並且LDH的存在有助於從Ag表面除去吸附的OH。此外，這樣的修飾策略增強Ag奈米粒子的分散，並顯著增加可利用的位點數量。Ag和LDH之間的協同作用顯著增強了ORR的催化活性。有趣的是，通過引入Ru和Ag NP，一方面改善LDH的本質上較差的導電性，另一方面通過這樣的設計可使LDH結構紊亂和產生缺陷位置（包括金屬和氧空位），因此調節Ni位點上的固有性質。這反過來又可增強用於OER上的位置活性及位點數量。Ag NP和LDH間的強協同作用分別在ORR和OER的雙功能電催化劑中設計Ag和Ni上的活性位點活性和群體。所製備的Ag NP/NiRu-LDH在鹼性OER和ORR上均顯示出極好的催化活性，其中起始過電位分別為0.21 V和-0.27 V，而OER和ORR之間的過電壓差為0.76 V，並具有出色的耐久性，證明了迄今報導的卓越的雙功能電催化劑。這項工作提供了一種新策略，以改善LDH的內在特性和工程多元化，以增強與電催化劑的整體雙功能活性相關的位點活性和群體。
第二項研究（第5章）為“在導電銀奈米線（Ag NWs）上生長3D NiMn層狀雙氫氧化物（NiMn-LDHs），以核殼結構之概念作為有效的ORR/OER雙功能電催化劑。因此，分層3D結構化的Ag NW@NiMn-LDHs催化劑在鹼性條件下表現出極好的OER / ORR活性。 Ag NW@NiMn-LDHs的突出的雙功能活性主要歸因於LDHs殼的分層3D開孔結構的協同貢獻，改善的電導率和與更易接近的位點群相關的LDH殼的小厚度。此外，Ag核與LDH殼金屬之間的電荷轉移效應，形成較少配位的Ni和Mn位點導致缺陷和變形位點，其強烈調節位點活性的本質活性，從而獲得增強的催化活性。因此，Ag NW@NiMn-LDH混合物在ORR和OER之間表現出0.75V的過電壓差，具有優異的耐久性30小時，證明了迄今為止報導的顯著的雙功能電催化劑。因此，Ag NW@NiMn-LDHs的分層3D架構的概念大大推進了對水電解和氧電催化劑的綜合研究。
本論文的第三種方法（第6章）是研究鹼性OER反應機制，利用臨場光譜電化學技術探測OER過程中NiMn-LDHs和β-Ni(OH)2電催化劑的活性位點和表面性質。鎳基層狀雙氫氧化物（LDHs）材料是高活性且具有成本效益的電催化劑，可用於高效析氧反應，並廣泛用於可持續發電。然而，在OER操作期間，真實活性位置和在Ni基LDH材料表面上發生的過程的機制尚不清楚。藉由臨場拉曼光譜的證據表明，隨著電極電壓的增加，NiMn-LDHs和β-Ni(OH)2中的Ni(OH)2相被氧化成NiOOH物質（對於NiMn-LDHs而言，在1.364 V以上）在實際水氧化之前，β-Ni(OH)2和NiOOH中間物質的1.464 V去質子化並帶電（“活性氧”），因此充當OER的前體。因此，我們提出“活性氧”物種的特性是鎳超氧化物或過氧化物性質。臨場X光吸收光譜提供證據表明，當電極電位增加時，Ni K-edge顯著轉移到更高的能量，表明NiMn-LDH中的Ni(OH)2氧化轉變為NiOOH，陽極氧化後構成催化OER所具備的活性位置。Ni K-edge的臨場EXAFS光譜表明，隨著施加的電極電位隨著新的形成而增加，屬於Ni(OH)2的Ni-O（R = 1.53 Å）和Ni-M（R = 2.73 Å）配位的強度逐漸減小。當電極電位越高時，在1.44 Å和2.42 Å處的峰分別對應於Ni3+周圍的Ni-O和Ni-M的配位數，表明由於Ni(OH)2向NiOOH的氧化轉變而在不同環境中存在形成新結構相。有趣的是，在不同電位下收集的Mn K-edge的臨場XANES光譜幾乎不變，FT-EXAFS的強度和峰位置保持不變，表明在OER過程中Mn位點沒有產生轉變。因此，我們得出結論，儘管在引入Mn時催化活性得到改善，但NiMn-LDHs在該應用上沒有顯示出平均Mn氧化態和配位數的任何變化。然而，NiMn-LDHs的Ni K-edge光譜隨施加電位顯著變化。因此，Ni構成活性中心並且顯然是OER的活性位點，而Mn原子的引入促進OER活性的協同作用。
另外，我們還使用臨場光譜電化學技術結合臨場XRD測量，在OER過程中對客體陰離子對NiMn-LDHs和Ni(OH)2催化劑的活性位點數和位點活性的影響進行了系統研究。反過來用於探測OER過程中的活動位點和結構變化。顯然，在引入客體陰離子（溴化物和氯化物）後，NiMn-LDHs表現出令人難以置信的OER活性，隨著客體陰離子濃度的增加，OER活性逐漸增加。這些觀察結果表明，由於LDHs結構的層間空間的擴展（通過臨場XRD測量證實），活性位點活性源自較少堆積和豐富的暴露的活性邊緣位點，促進了OER活性。與NiMn-LDHs不同，Ni(OH)2/NiOOH的氧化還原轉變和β-Ni(OH)2催化劑的OER活性在引入客體陰離子後受到顯著影響並被抑製到更高的過電位。這些結果表明，由於β-Ni(OH)2在結構上緊密堆積，客體陰離子只有一種與Ni(OH)2相互作用的可能性，並且正在攻擊Ni位點，這推測是OER活性下降的原因。
通過修飾和核殼結構的策略將LDH與導電Ag NP和Ag NW結合在一起，設計具結構無序和缺陷的觸媒，從而在鹼性OER和ORR操作期間增強其導電性、活性及穩定性。所討論的具有高OER活性的NiMn-LDHs催化劑，其臨場光譜電化學表徵表明Ni位點為活性中心，而Mn的存在為促進OER活性的協同作用。儘管目前的研究僅限於研究LDH用於氧電催化的活性位點和表面性質，但這些考慮也預期延伸到其他LDHs催化劑和電化學反應

Developing advanced nanomaterials and catalytically active materials is a substantial area of research to meet the growing global energy demand, given the central role that electrocatalytic reactions play in green sustainable energy generation, storage and conversion. However, development of catalytically active, operationally stable and inexpensive materials for the bifunctional oxygen evolution (OER) and reduction reaction (ORR) is one of the grand challenges in renewable energy storage and conversion technologies such as metal-air batteries and fuel cells due to the sluggish reaction kinetics of OER and ORR even when noble metal catalysts such as platinum with carbon support (Pt/C for ORR), ruthenium oxide (RuO2), and iridium oxide (IrO2) toward OER are applied. Consequently, a critical feature is to develop robust materials that have outstanding catalytic activity, cost-effective and promising durability for the more difficult ORR/OER process.
Currently, transition metal hydroxides/oxides and Ni-based layered double hydroxides (LDHs) electrocatalysts are an interesting alternative to the novel metal-based electrodes in alkaline solutions due to their low cost, abundance, proven ability to catalyze the OER/ORR and operationally stable in high pH values of the electrolytes. To accelerate the development of Ni-based LDHs electrocatalysts with improved catalytic activities for the OER/ORR, it is essential to increase the understanding of the mechanisms, active sites at a fundamental level, and surface properties at relevant potentials during the OER and ORR operation and remains of great importance to the design of new electrocatalysts.
This dissertation aims to develop endurable, inexpensive, and efficient bifunctional electrocatalysts for the OER and ORR operated under alkaline conditions at room temperature; investigate the mechanisms, active sites, and surface properties during the OER process using in situ spectro-electrochemical techniques. Accordingly, new classes of Ni-based LDHs electrocatalysts (NiRu-LDHs and NiMn-LDHs nanosheets) were developed and integrated with conductive supports (silver nanoparticles (Ag NPs) and silver nanowires (Ag NWs)) using decoration action and core-shelling strategies as efficient bifunctional electrocatalysts for OER and ORR. This approaches will have great benefits to design highly active and stable bifunctional electrocatalysts for the next-generation reversible oxygen electrodes involve the combination of less-expensive single-function OER and ORR electrocatalysts into one hybrid system.

The first approach (Chapter 4) investigated in this dissertation “Site activity and population engineering of NiRu-layered double hydroxide nanosheets decorated with conductive silver nanoparticles for oxygen evolution and reduction reaction”. This work focuses on the development of new electrocatalyst; NiRu-LDHs decorated with Ag NPs (Ag NP/NiRu-LDHs) as efficient and stable bifunctional electrocatalyst toward the OER and ORR and intended to distinguish the site activity and site population associated to the overall catalytic activity. The higher ORR activity of Ag NP/NiRu-LDHs was mainly attributed to the increased Ag site activity and accessible Ag site populations. The increased Ag site activity is extensively contributed from the charge polarization occurring on the Ag sites responsible for weakening the adsorption of OH on the Ag sites and the presence of LDHs helps to remove the adsorbed OH from the surface of Ag. Furthermore, the decoration strategy enhances the dispersion of Ag and considerably increased the accessible site populations. These strong synergetic effects between Ag and LDHs significantly enhanced the catalytic activity of the ORR. Interestingly, engineering multiple vacancies (metal and oxygen vacancies) which causes the structural disorder and defects through the introduction of Ru and decorating NiRu-LDHs nanosheets with conductive Ag NPs (improve the intrinsically poor conductivity of LDHs) tunes the intrinsic properties of the Ni sites which in turn enhances the OER site activity and site populations. The strong synergetic effects of silver nanoparticles and metal LDHs engineer the active site activity and populations on both Ag and Ni in the bifunctional electrocatalysts for ORR and OER, respectively. The as-prepared Ag NP/NiRu-LDH shows substantially marvelous catalytic activity toward both OER and ORR features with low onset overpotential of 0.21 V and -0.27 V, respectively, with 0.76 V overvoltage difference between OER and ORR with excellent durability, demonstrating the preeminent bifunctional electrocatalyst reported to date. This work provides a new strategy to improve the intrinsic properties of LDHs and engineering multivacancies to enhance the site activity and populations associated with the overall bifunctional activity of the electrocatalysts.

The second study (Chapter 5) aims to develop “hierarchical 3D NiMn-layered double hydroxide (NiMn-LDHs) shells grown on conductive silver nanowires (Ag NWs) cores as efficient ORR/OER bifunctional electrocatalysts”. As a result, the hierarchical 3D architectured Ag NW@NiMn-LDHs catalysts exhibit superb OER/ORR activities in alkaline condition. The outstanding bifunctional activities of Ag NW@NiMn-LDHs are essentially attributed to the synergistic contributions from the hierarchical 3D open-pores structure of the LDHs shells, improved electrical conductivity and small thickness of the LDHs shells associated to more accessible site populations. Moreover, the charge transferring effect between Ag cores and metals of LDHs shells, the formation of less coordinated Ni and Mn sites causes defective and distorted sites that strongly tune the intrinsic activity of the site activity and hence attaining enhanced catalytic activities. Thus, Ag NW@NiMn-LDH hybrids exhibit 0.75 V overvoltage difference between ORR and OER with excellent durability for 30 h, demonstrating the distinguished bifunctional electrocatalyst reported to date. Thus, the concept of the hierarchical 3D architecture of Ag NW@NiMn-LDHs considerably advances comprehensive research towards water electrolysis and oxygen electrocatalyst.

The third approach (chapter 6) of this dissertation is to investigate the mechanisms, probe the active sites and surface properties of NiMn-LDHs and β-Ni(OH)2 electrocatalysts during the OER operation using in situ spectro-electrochemical techniques. Ni-based layered double hydroxides (LDHs) materials are highly active and cost-effective electrocatalysts that can be potentially used for efficient water oxidation process and extensively used toward sustainable energy generation. However, the mechanisms at a fundamental level, active phases and the processes occurring on the surface of Ni-based LDHs materials during the OER operation are not clearly known. Accordingly, the evidence from in situ Raman features provide that the Ni(OH)2 phases in both NiMn-LDHs and β-Ni(OH)2 get oxidized to NiOOH species as the electrode voltage increasing and NiOOH intermediate species deprotonated and get charged prior to the real water oxidation, suggesting that the formation of “active oxygen” species and hence acts as a precursors for the OER. We therefore propose that the identity of the “active oxygen” species is nickel superoxidic or peroxidic nature. The in situ XANES spectra provides the evidence that the Ni K-edge significantly shifted to higher energy upon the electrode potential increased, suggesting the redox transition of Ni(OH)2 in NiMn-LDHs to NiOOH upon anodization that constitutes the catalytic activity of OER active center. The in situ EXAFS spectra of Ni K-edge indicates that the intensity of both Ni−O (R =1.53 Å) and Ni−M (R =2.73 Å) coordination spheres gradually decreases as the applied electrode potentials increase prior to the OER whereas the formation of new peaks at 1.44 Å and 2.42 Å corresponding to the coordination sphere of Ni−O and Ni−M, suggesting the formation of new phases existing in different environment due to the redox transition of Ni(OH)2 to NiOOH occurs. The intensity of these peaks substantially increased as the voltage of electrode increased. However, the intensity and peak positions of Mn K-edge collected at different potentials are almost similar and remain unchanged, suggesting no transformation of Mn sites during the OER process. We therefore conclude that Ni constitutes the active center and evidently the active site for the OER whereas the introduction of Mn atom promotes synergistically the OER activity. We also present a systematic studies of guest anion effect on the number of active sites and site activity of NiMn-LDHs and Ni(OH)2 catalysts during the OER process using electrochemical, in situ spectro-electrochemical techniques and in situ XRD measurements, which in turn used to probe the active sites and structural change during the OER process. Evidently, the NiMn-LDHs exhibited incredible OER activity after guest anions (bromide and chloride) introduced and the OER activity gradually increased as the concentration of guest anions increased. These observations suggest that the active site activity originated from the less-stacking and plentiful exposed active edge sites due to the expansion of interlayer spaces of LDHs structure (confirmed by the in situ XRD measurement) promotes the OER activity. Unlike NiMn-LDHs, both the redox transition of Ni(OH)2/NiOOH and the OER activity of β-Ni(OH)2 catalyst is significantly affected after guest anions introduced and suppressed to higher overpotential. These results suggest that since β-Ni(OH)2 is structurally close-packed, the guest anions have only one possibility to interact with Ni(OH)2 and that is attacking the Ni sites which certainly accounts for the declined OER activity.

In general, integrating LDHs with conductive Ag NPs and Ag NWs through decoration and core-shelling strategies engineers multiple vacancies which cause the structural disorder and defects essentially enhances bifunctional properties of the hybrids, conductivity, stability during OER and ORR operation. The discussed in situ spectro-electrochemical characterization of NiMn-LDHs catalysts with high OER activity demonstrates that the Ni sites constitute the active center and the presence of Mn atom promotes synergistically the OER activity. Although the recent studies are limited to investigate the active sites and surface properties of LDHs for oxygen electrocatalysis, these considerations are also anticipated to extend to other LDHs catalysts and electrochemical reactions.

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