Title Page
Contents
ABBREVIATIONS 12
ABSTRACT IN KOREAN 14
PART I. A brief literature review of single-entity electrochemistry of soft particles with use of chronoamperometry technique and working ultramicroelectrode 17
1.1. Introduction of the single-entity electrochemistry (SEE) concept 17
1.2. Behaviors of entities in their SEE collision events. 22
1.2.1. Electrical conduction 22
1.2.2. Direct reaction 24
1.2.3. Blockage 26
1.2.4. Electrocatalysis 28
1.3. The SEE research of soft particles in literature 30
1.3.1. Solid NPs 30
1.3.2. Liquid NPs 33
1.3.3. Bio-entities 36
1.4. Summary and orientation for research practice 40
PART II. Electrosynthesis of palladium nanocatalysts using single droplet reactors and catalytic activity for formic acid oxidation 43
2.1. Introduction 43
2.2. Experimental 45
2.2.1. Materials 45
2.2.2. Instrumentation 46
2.2.3. Preparation of UMEs 46
2.2.4. Preparation of Pd2+ emulsions[이미지참조] 46
2.2.5. Electrochemical experiments 47
2.3. Results and discussion 47
2.3.1. Electrochemical behavior of Pd2+ in aqueous solution phase on carbon substrate[이미지참조] 47
2.3.2. Characterization and stability of Pd2+ emulsions[이미지참조] 50
2.3.3. Quantifiable SEE synthesis of monometallic Pd 52
2.3.4. Characterization of the Pd products 57
2.3.5. Catalytic activity of the synthesized Pd for formic acid oxidation 61
2.4. Conclusion 68
PART III. Detection of individual conjugated polyelectrolyte (CPE) entities through their catalytic activity for a solution-phase redox species 69
3.1. Introduction 69
3.2. Experimental 73
3.2.1. Materials 73
3.2.2. Instrumentation 74
3.2.3. Preparation of UMEs 74
3.2.4. Preparation of CPE aqueous solutions 75
3.2.5. Electrochemical experiments 75
3.3. Results and discussion 76
3.3.1. Choosing an inert WE substrate with a given potential redox indicator 76
3.3.2. Testing the Pi CPEs electrochemical behaviors with employments of the potential WE substrate and potential redox indicator 77
3.3.3. Characterization of the Ps suspension by DLS method 83
3.3.4. SEE of P5 CPE and the characterization of P5 suspensions[이미지참조] 86
3.4. Conclusion 90
REFERENCES 92
ABSTRACT IN ENGLISH 110
Table 1.1. Summary of some soft material investigated in literature with the... 42
Table 2.1. Predicted average radii of Pd nanocatalysts formed in one deposition event... 59
Table 2.2. The mass activity data of synthesized Pd nanocatalysts following the... 65
Table 2.3. Comparison of the catalytic activities of different synthesized Pd-based... 66
Figure 1.1. The SEE and ECL combined... 21
Figure 1.2. Conducting collision of reduced graphene oxide (rGO) on the working... 23
Figure 1.3. Illustration of collision entity directly reduces... 25
Figure 1.4. Two emulsion droplet reactors, NB containing TCNQ (top) and pure NB... 26
Figure 1.5. Illustration of collision entity blocks the... 27
Figure 1.6. Illustration of collision entity electro-... 28
Figure 1.7. Models of SEE collision events of some different carbonaceous... 32
Figure 1.8. Schematic illustration of some typical SEE research of emulsion droplets... 35
Figure 1.9. Schematic diagrams of the SEE detections of some differentiated bio-... 39
Figure 2.1. Schematic illustration of Pd nanocatalysts synthesis and formic acid oxidation. 45
Figure 2.2. (A) Overlay of the CVs recorded with a 7 ㎛ C-UME and a Ag/AgCl RE... 50
Figure 2.3. (A) Pictures of the Pd2+ emulsions with the Pd2+ concentrations of 0, 5,...[이미지참조] 51
Figure 2.4. The representative i-t records of the emulsion... 52
Figure 2.5. Respective overlays for comparisons of droplet size distributions... 55
Figure 2.6. SEM-EDS images of Pd-deposited C-UME surface at the edge (A) and... 61
Figure 2.7. CVs recorded in a 0.5 MHCOOH + 0.25 M H₂SO₄ solution... 63
Figure 2.8. The mass activities of the synthesized Pd nanocatalysts along with the... 66
Figure 2.9. CV result for ECSA determination of the synthesized Pd nanocatalyst... 67
Figure 3.1. Illustrations of Pi CPEs. (A) Pictures of the stock Pi CPEs of...[이미지참조] 72
Figure 3.2. Molecular structure of AB. 72
Figure 3.3. Schematic illustration of CPE cluster collision catalyzing for AB... 73
Figure 3.4. Overlays of CV curves recorded at... 77
Figure 3.5. (Left) Overlays of CV curves recorded at scan rate 0.1 V/s with 3 mm d.... 78
Figure 3.6. Overlays of CV curves recorded with 10 ㎛ C-... 83
Figure 3.7. (A) The pictures of the(filtered) P5 CPE...[이미지참조] 85
Figure 3.8. (A) The i-t records in the SEE detections of P5 entities in the solutions...[이미지참조] 87
Figure 3.9. Transfer of a charge carrier(a positive polaron) between CPEs chains... 90