Functional Morphology of Metal Core and Ti1-XMoXOy Nanosupports for Pt Nanocrystals toward Oxygen Reduction Reaction

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研究生：	NGUYEN TRUNG THANH NGUYEN - TRUNG THANH
論文名稱：	Functional Morphology of Metal Core and Ti1-XMoXOy Nanosupports for Pt Nanocrystals toward Oxygen Reduction Reaction Functional Morphology of Metal Core and Ti1-XMoXOy Nanosupports for Pt Nanocrystals toward Oxygen Reduction Reaction
指導教授：	黃炳照 BING-JOE HWANG
口試委員:	劉炯權劉炯權周澤川周澤川杜景順杜景順蘇威年蘇威年楊明長楊明長
學位類別：	博士 Doctor
系所名稱：	工程學院 - 化學工程系 Department of Chemical Engineering
論文出版年：	2012
畢業學年度：	101
語文別：	英文
論文頁數：	246
中文關鍵詞：	Pt nanocrystals 、functional metal and oxide supports 、oxygen reduction reaction 、PEMFC.
外文關鍵詞：	Pt nanocrystals, functional metal and oxide supports, oxygen reduction reaction, PEMFC.
相關次數：	點閱：393 下載：3
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Fuel cell technology is a promising solution for the energy issues over the world. Among the wide variety of fuel cells, Proton Electrolyte Membrane Fuel Cells (PEMFCs) are highly regarded by scientists as a non-polluting power source with good commercial viability. The main objective in fuel cell technologies is to develop low-cost, high-performance and durable materials. However, current fuel cell systems have high intrinsic costs and fairly poor durability. For PEMFCs, the improvements both of catalytic activity and stability of Pt nanocrystals for oxygen reduction reaction (ORR) are the prerequisite issues before PEMFCs can be commercialized for automotive applications. Previous reports showed that the ORR is kinetically limited at the cathode and the
instability of Pt on the cathode is marked by the loss of Pt electrochemical surface area (ECSA)over time, due to Pt dissolution/aggregation/Oswald ripening - these being the major contributors to the degradation of fuel cell performance. Additionally, the predominance of weak interactions between the carbon support and the catalytic metal nanoparticles leads to the sintering of the catalytic metal nanoparticles and a consequent decrease in the active surface area with long-term operation. More importantly, the high potentials that accelerate both electrochemical carbon corrosion and the dissolution of the active elements under normal operating conditions, are issues impacting on fuel cell durability that remain unresolved. Therefore, this dissertation is focused on the "Functional morphology of metal core and Ti1-XMoXOy nanosupports for Pt nanocrystals toward oxygen reduction reaction". This is a collection of new selected approaches for enhancing ORR performance of Pt nano-electrocatalysts.
1) The first approach is entitled: "Functional Pd tetrapod core of heterogeneous Pd-Pt nanodendrites for enhancing oxygen reduction reaction". Herein, the Pd tetrapod core is demonstrated to effectively enhance the catalytic activity and durability of Pd@Pt nanodendites for the ORR. Special attention is given to the positively coupled effect of oxalate ion-formaldehyde during the hydrothermal synthesis of various Pd morphologies at different temperatures. To be able to synthesize tetrapodal morphology in an aqueous solution, the (110) and (111) planes on truncated tetrahedral Pd seeds are passivated at 150 oC by the adsorption of oxalate ions and CO, a product from the decomposition of formaldehyde on crystalline Pd surfaces. However, Pd nanotetrahedra can be obtained at 200 oC, due to the weakened effect of CO and oxalate ions. Thus,
Pd tetrapod synthesis can be achieved by selective deposition of fresh Pd atoms onto (100) planes of truncated tetrahedral Pd seeds without directly using hazardous CO gas. Pt (30 wt%) on tetrapodal and truncated octahedral Pd cores and Pt (50 wt%) on tetrapodal Pd cores were compared against commercial Pt/C (E-Tek) for ORR. The Pdtetrapod@30 wt% Pt catalyst exhibited the highest ORR catalytic activity. Overall, the Pd tetrapod core has a functional morphology
which offers high-index facets for the subsequent deposition of Pt(110)nanodendrites and the bimetallic interaction between two materials allows good electron transfer from Pd core into Pt surfaces. Both effects contribute to increased catalytic activity of Pdtetrapod @30 wt% Pt, even under a lower loading of Pt. Pdtetrapod @30 wt% Pt has rather large particle size (~39.5 nm) which exhibits excellent durability and resistance to the agglomeration or sintering of Pt.
2) The second approach is entitled: "Synthesis of Ti0.7Mo0.3O2 supported-Pt nanodendrites and their catalytic activity and stability for oxygen reduction reaction". This part shows that the integrated material of robust non-carbon Ti0.7Mo0.3O2 nanosupports and Pt dendritic layer was demonstrated to effectively enhance the activity and stability of Pt nano-electrocatalysts for the ORR. Hetero-nanostructural clusters (HNC) of Ptd/Ti0.7Mo0.3O2 were synthesized by a simple aqueous-phase route, in which the deposition and growth of Pt nanoparticles were controlled to obtain high-index facets of Pt. In the synthesis, Pt4+ ions were reduced and formed nuclei in the presence of L-ascorbic acid and Cetyltrimethylammonium bromide (CTAB). With adequate control of dosage intervals and temperature, the following addition of Pt precursor solution was carried out by injecting the precursor into the suspension solution containing Ti0.7Mo0.3O2. The clustering of Pt particles could be driven by their high surface energy due to a large surface area to-volume ratio. 20 wt% Ptd/Ti0.7Mo0.3O2-HNC and support-free Pt nanodendrite catalysts were prepared and compared against commercial 20 wt% Pt/C (E-TEK) for ORR. TEM, XRD, X-ray Absorption Near Edge Structure (XANES), and electrochemical techniques were applied to characterize these catalysts. Effects of high index facets on dendritic Pt surface contribute to the enhanced catalytic activity and stability of Ptd/Ti0.7Mo0.3O2-HNC towards the ORR. In addition,electron transfer originating from strong metal-support interactions (SMSI) and corrosion-resistant Ti0.7Mo0.3O2 nanosupport also play important roles.
3) The final approach is entitled: "Defect-Structural Ti0.9Mo0.1Oy Supported-Pt nanocrystals Used as High-Performance Catalyst for Oxygen Reduction Reaction". The search for catalysts with high activity and longer-term stability for ORR in PEMFC is ongoing. In this research, we investigated the idea that advanced defect structural Ti0.9Mo0.1Oy nanosupports significantly enhanced the ORR activity and stability of supported-Pt catalysts. Here the approach of synthesis
involves anchoring of Pt(111) nanoparticles on the defect structural Ti0.9Mo0.1Oy nanosupports (d-Ti0.9Mo0.1Oy). While the structural defects of Ti0.9Mo0.1Oy are made by doping Molybdenum into anatase-TiO2 structure and Hydrogen-treatment at a high temperature (300 oC). The structural defects of this material were studied by Kroger-Vink defect theory, density functional theory (DFT)calculations, and examined by the experimental Raman, electronic conductivity measurements.Rotating disk electrode (RDE) measurements showed that 20 wt% Pt/d-Ti0.9Mo0.1Oy catalyst had 1.5 times and ∼ 9.1 times higher Pt mass activity for ORR than those of 10 wt% Pt/d-Ti0.9Mo0.1Oy and commercial Pt/C catalysts, respectively. The observed high activity of metal oxide supported-
Pt catalyst is attributed to the role of the advanced oxide support with electron donation from support to Pt catalyst surface, oxygen vacancies on nanosupport surface and high conductivity. Pt nano-electrocatalysts on the advanced robust non-carbon d-Ti0.9Mo0.1Oy nanosupports also exhibits improved stability against Pt sintering under a potential cycling regime (3000 cycles from 0.4 V to 1.0 V vs. RHE) due to SMSI. Moreover, the role of oxygen vacancies on oxide surface was also investigated as a means to enhance ORR activity by DFT theory.
This collection of new approaches not only provides feasible paths for enhacing the efficiency of PEMFCs but also extends different catalysis reactions such as CO oxidation, hydrogenation,methanol oxidation reaction in DEMFCs etc., or in different applications including biosensors,optical materials (on tetrapod morphology of Pd-based materials) etc.

Abstract ........................ I
Acknowledgement .................. V
Table of Contents ................ VI
List of Schemes ...................XIII
List of Figures .................... XIV
List of Abbreviations ............... XXIX
Chapter 1. Introduction and current challenges for Proton exchange membrane fuel cells .... 1
1 Overview about fuel cell technology ................ 1
2 Proton exchange membrane fuel cells (PEMFC) ......... 4
2.1 Overview about PEMFC .............................. 4
2.2 The operating principle of PEMFCs ................ 6
3 Current challenges for PEMFCs ....................... 9
3.1 Degradation and durability issues in catalyst layers ......... 9
3.1.1 Platinum degradation .............................. 9
3.1.2 Carbon support degradation ........................ 14
3.1.3 Ionomer degradation and interfacial degradation ............ 18
3.2 Cost of Pt metal catalyst .............................. 19
3.3 ORR activity issues ......................................... 20
3.4 Carbon-support oxidation ............................ 22
Chapter 2. Morphologies-controlled Pt based nanocrystals and Bimetallic Pd-Pt
nanodendrite for Oxygen Reduction Reaction .................... 24
1 Introduction ........................ 24
2 Morphologies and Fuel cell applications of metal nanocrystal ......... 24
3 Synthesis methods and effects to quality of size- and shape-nanoparticles ................... 27
3.1 Synthesis methods for metal nanocrystals ................. 27
3.1.1 Reduction methods....... 27
3.1.2 Thermal decomposition methods ...................... 29
3.2 Effects to quality of size and shape particle for metal nanocrystals ............................... 30
3.2.1 Nucleation and growth-size control of noble metal nanoparticles ........................... 30
3.2.2 Shape control and Effects to quality of shape-nanoparticles ...... 34
4 The examples of shape control and mechanism for preparation of Pd and Pt based nanocrystals ........................... 53
4.1 Formation of polyhedrons ............................. 54
4.2 Concave metal nanocrystals ........................... 56
4.2.1 Amine-Assisted Synthesis of Pt Nanocrystals with High-Index Facets .................. 56
4.2.2 Concave Pd Polyhedra with Controllable Concavity.......... 60
4.3 Nanorods and nanowires.............................. 63
4.4 Preparation of Ultrathin Pd Nanosheets Aided by Carbon Monoxide .... 66
4.5 Multi-branches and nanodendrite materials ........... 71
4.5.1 Multipods from Nanocrystal Overgrowth ............. 71
4.5.2 Dendrite and branch Pt-based nanocrystals .......... 75
5 Bimetallic Pt-based nanodendrite for fuel cells ....... 84
Chapter 3. Non-Carbon Support materials of Pt nano-electrocatalyst for fuel cells .............. 88
1 Support materials of Pt nano-electrocatalyst for fuel cells ........ 88
2 Non-carbonaceous and inorganic oxide/carbide supports ............... 92
2.1 Ti-based compounds ................... 93
2.1.1 Titanium oxides (TiO2-x or TinO2n-1) ................. 93
2.1.2 Titanium nitride (TiN) ............................ 98
2.1.3 Titanium diboride (TiB2) .................. 99
3 Other dopants for Titania ................ 100
Chapter 4. Material and methods ............... 103
1 Materials ............. 103
2 Methods ................. 103
2.1 X-ray diffraction (XRD) measurements ................ 103
2.2 Transmission electron microscopy (TEM) measurements ............. 103
2.3 Determining of metal(s) loading ................ 103
2.4 Surface area measurement .................... 104
2.5 Electronic conductivity measurement ............ 104
2.6 X-ray absorption spectra (XAS) measurement ................. 104
2.7 Raman measurements .................... 104
2.8 Oxygen-vacancy concentration calculation .............. 105
2.9 DFT simulation to model Ti1-xMoxOy, Pt/d-Ti1-xMoxOy structures and oxygen adsorption on Pt and oxygen vacancy sites ....... 105
2.10 Electrode preparation and electrochemical measurements ......... 106
Chapter 5. Functional Pd tetrapod core of heterogeneous Pd-Pt nanodendrites for enhancing oxygen reduction reaction ........... 108
1 Introduction .................... 108
2 Experimental section.............. 110
2.1 Synthesis of Pd cores ............ 110
2.1.1 Synthesis of Pd nanocubes ............... 110
2.1.2 Synthesis of Pd truncated octahedrons .............. 111
2.1.3 Synthesis of Pd tetrapods ....................... 111
2.2 Synthesis of Pd-Pt bimetallic nanocrystals with the dendritic shell ............................. 112
3 Results and discussion ................... 112
3.1 Structure of Pd nanotetrapods ......................... 112
3.3. Formation mechanism of Pd nanotruncated octahedra, tetrahedra, and tetrapods ...... 115
3.4 Pt nanodendrites on various Pd core morphologies ............... 117
3.5 Electrocatalytic activity and stability toward the ORR ......... 120
3.6. The functional morphology of Pd cores for the ORR performance enhancements ..... 122
4 Conclusions .................... 125
Chapter 6. Synthesis of Ti0.7Mo0.3O2 supported-Pt nanodendrites and their catalytic activity and stability for oxygen reduction reaction ........ 126
1 Introduction ............................ 126
2 Experimental section...... 128
2.1. Synthesis of Ti0.7Mo0.3O2 nanoparticles ...... 128
2.2. Synthesis of Ptd/Ti0.7Mo0.3O2 nanodendrite clusters .......... 128
3. Results and discussion .......... 129
3.1. Characterization of Ti0.7Mo0.3O2 support material ........... 129
3.2. Characterization of Ptd/Ti0.7Mo0.3O2 catalysts and the formation mechanism of dendritic Pt layer on Ti0.7Mo0.3O2 nanosupports............. 130
3.3 Electrochemical performances of Pt catalysts .......... 134
Chapter 7. Defect-Structural Ti0.9Mo0.1Oy Supported-Pt nanocrystals Used as High-Performance Catalyst for Oxygen Reduction Reaction ........... 140
1 Introduction ............................... 140
2 Experimental section.................. 142
2.1 Synthesis of Ti1-xMoxOy nanoparticles .................. 142
2.2 Synthesis of the defect structural Ti0.9Mo0.1Oy (d-Ti0.9Mo0.1Oy) nanosupport ............. 142
2.3 Deposition of Pt nanoparticles onto the d-Ti0.9Mo0.1Oy nanosupports .......................... 142
3 Results and discussion .................. 143
3.1 Characterization of Ti0.9Mo0.1Oy ......................... 143
3.1.1 XRD measurements .................................. 143
3.1.2 Raman and X-ray adsorption spectroscopy (XAS) measurements .... 144
3.1.3 TEM and TEM mapping images of Ti0.9Mo0.1Oy materials ........ 146
3.1.4 Defect structure Ti1-xMoxOy materials ............... 147
3.1.5 Characterization and oxygen-vacancy concentration of d-Ti0.9Mo0.1Oy materials.... 149
3.2 Characterizations of Pt/d-Ti0.9Mo0.1Oy and Pt/C (E-TEK) samples ............................. 152
3.2.1 TEM measurements ............................. 152
3.2.2 X-ray absorption fine structure studies ............. 153
3.3 Electrochemical behavior of d-Ti0.9Mo0.1Oy nanosupports and Pt/d-Ti0.9Mo0.1Oy nanocrystals............. 154
3.4 Oxygen vacancies promote the ORR activity enhancement of Pt/d-Ti0.9Mo0.1Oy catalysts.Computation results .... 158
4 Conclusions ................................. 159
Chapter 8. Summary and conclusions ......................... 161
Supporting information .................................. 163
References ........... 177
CURRICULUM VITAE .......... 215
List of publications ............................ 216
List of conferences.................. 217

                                

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