Fabrication of solid state supercapacitors by inkjet printing

THAI NGUYEN UNIVERSITY UNIVERSITY OF AGRICULTURE AND FORESTRY NGUYEN CHI CONG FABRICATION OF SOLID STATE SUPERCAPACITORS BY INKJET PRINTING BACHELOR THESIS Study mode: Full-time Major: Environmental Science and Management Faculty: Advanced Education Program Office Batch: 2014-2018 Thai Nguyen, 25/09/2018 DOCUMENTATION PAGE WITH ABSTRACT Thai Nguyen University of Agriculture and Forestry Degree Program Student name Studen ID Bachelor of Environmental Science and Management Nguyen Chi Cong DTN1454290005 FABRICATION OF SOLID STATE SUPERCAPACITORS Thesis Title BY INKJET PRINTING Prof Kuan-Jiuh Lin – National Chung Hsing University, Taiwan Supervisor(s) Dr Nguyen Thanh Hai – Thai Nguyen University of Agriculture and Foresttry, VietNam Abstract: CNT ink and MnO2 ink were produced to fabricate solid state supercapacitor electrodes through contactless deposition We used inkjet printing technology to deposit CNTs on photo paper to produce a conductive film of 500 Ω/sq., followed by depositing manganese dioxide on the conductive film to enhance its capacitive properties The electrochemical properties of CNT/MnO2 were significantly improved, and the most complete CNT/MnO2-20 capacitance value in the structure was 431.25 μF/cm2, which is nearly 3.5 times as high as that of CNT with 125.52 μF/cm2 In addition, the capacitor system adopts solid electrolyte This type of electrolyte is free from danger of liquid leakage, therefore the packaging cost will be reduced Key-words: Ink jet printing; Solid state supercapacitor; CNT/MnO2 i nanowire; Carbon nanotube; Contactless deposition Number of pages: 59 Date of submission: 25th September, 2018 Supervisor’s signature ii ACKNOWLEAGEMENT First of all, I would like to thank the coperation between Thai Nguyen University of Agriculture and Forestry and National Chung Hsing University for providing me an amazing opportunity to conduct my internship in Taiwan It brings me great pleasure to work and submit my thesis for graduation It is my pleasure to work with a profound supervisor - Professor Kuan-Jiuh Lin whose guidance, encouragement, suggestion and very constructive criticism have contributed immensely to the evolution of my idea during the project Without his guidance, I may not have this thesis I sincerely thank Dr Nguyen Thanh Hai for his advices, assistance, sharing experiences before and after I went to Taiwan, helping me to understand and complete my proposal and thesis He also helped me a lot by spending much time for checking my thesis report I consider it is an honor to work with Mr Wu, an exceptional master student, who is particularly helpful in guiding me toward a qualitative methodology and inspiring me in whole period of internship time He is always helpful, friendly and very kind with me Without his guidance, I cannot accomplish this thesis Thank to Mr Lai and all the member in KJ lab who hearty helped me a lot when I worked in there I am really fortunate to be a member of Professor KuanJiuh Lin’s Laboratory Finally, I would like to express my deeply gratitude to my family and friends for providing me emotional, unceasing encouragement, physical and financial support I would like to thank all those other persons who helped me in completing this report iii Because of my lack knowledge, the mistake is inevitable, I am very grateful if I receive the comments and options from teachers and others to contribute my report Sincerely yours, Nguyen Chi Cong iv TABLE OF CONTENTS DOCUMENTATION PAGE WITH ABSTRACT i ACKNOWLEAGEMENT iii TABLE OF CONTENTS v LIST OF FIGURES vii LIST OF TABLES x LIST OF ABBREVIATIONS xi PART INTRODUCTION 1.1 Research rationale 1.2 Research’s objectives PART LITERATURE REVIEW 2.1 Supercapacitors review 2.1.1 Electric double-layer capacitors 2.1.2 Pseudo-capacitors 2.2 Carbon nanotube inkjet printing review 2.2.1 Carbon Nanotube Dispersion 10 2.3 Manganese dioxide 11 PART METHODS AND MATERIALS 15 3.1 Experimental Instruments 15 3.2 Experimental materials 16 3.3 Experimental methodology 16 3.4 Synthesis Methods 17 v 3.4.1 Preparation of CNT ink 17 3.4.2 Synthesis of MnO2 nanowires 17 3.4.3 Preparation of MnO2 ink 18 3.4.4 Single Electrode Production 18 3.4.5 Solid Electrolyte Production 18 3.4.6 Preparation of solid state Supercapacitor Devices 18 3.5 Material Characteristics Analysis 19 3.6 Measurement of super capacitor electrode elements 20 PART RESULTS AND DISCUSSION 22 4.1 Carbon Nanotube Synthesis and morphology identification 22 4.2 Synthesis of MnO2 nanowires 24 4.3 MnO2 NW printed on conductive substrate CNT 27 4.4 Identification of CNT/MnO2NW morphology 29 4.5 CNT/MnO2NW-5, 10, 20, 30 cyclic voltammetry 32 4.6 CNT/MnO2NW-20 Constant Current Charge and Discharge Cycle Test 34 4.7 Series Capacitor Charge and Discharge Test 40 4.8 Comparison of Literature 41 4.9 Long-cycles stability 42 PART CONCLUSION 43 REFERENCES 44 vi LIST OF FIGURES Figure 2.1 Power density and energy distribution of conventional capacitors, batteries, fuel cells, and supercapacitors (Source: Internet) Figure 2.2 Relationship between interface distance and potential between two conductors Figure 2.3 Electric double layer charge distribution model (a) Helmholtz model, (b) Gouy-Chapman model and (c) Stern model Figure 2.4 Carbon tubes and overlapping carbon tubes form an electron pathway 10 Figure 2.5 (a) α-Manganite; (b) β-Pyrolusite; (c) γ-Nsutite; (d) δ-Bismuthite; (e) Crystal structure of λ-Spinel and (f) ε-Ramsdellite phase of MnO2 13 Figure 2.6 CV curves for α, β, γ, δ, and λ-MnO2 in a 0.1 mol Na2SO4 electrolyte system 13 Figure 2.7 Electrochemical deposition MnO2 nanotubes (a) SEM Image and (b) in mol Na2SO4 in the electrolyte system, the current density is A/g , A/g , A/g , 10A/g charge and discharge curve 14 Figure 2.8 (a) TEM images of MnO2-MWCNTs composites and (b) Charge and discharge curves at current densities of 0.2 A/g, 0.5 A/g, and A/g, respectively, in a 0.5 mol Na2SO4 electrolyte system 14 Figure 3.1 Two electrode patterns and assembly 19 Figure 3.2 Bipolar device 19 Figure 3.3 Supercapacitor test equipment configuration 21 Figure 4.1 Surface resistance and SDS/MWCNT ratio 23 Figure 4.2 (a) and (b) Low-magnification and high-magnification SEM images of 0.2g CNT and 0.16g SDS on paper after being printed 20 time, (c) EDS spectrogram 23 Figure 4.3 (a) and (b) SEM images of MnO2 nanowires at a holding temperature of at 0.080M for 0.039M MnSO4 • H2O and 0.099M KMnO4 precursor solutions, (c) EDS spectrogram 24 vii Figure 4.4 Growth of MnO2 Nanowires 25 Figure 4.5 SEM images of MnO2 nanowires synthesized from 0.039M MnSO4•H2O and 0.1M KMnO4 precursor solutions at 180°C for 1h (a), 4h (b) and 12h (c) 26 Figure 4.6 XRD pattern of MnO2 nanostructures prepared by holding a solution of 0.039M MnSO4 • H2O and 1M KMnO4 precursors at 180°C for hour, hours and 12 hours 27 Figure 4.7 CNT/MnO2 NW Cyclic Voltammogram at low scan rates 29 Figure 4.8 CNT/MnO2 NW Cyclic Voltammogram at high scan rates 29 Figure 4.9 SEM image of CNT/MnO2NW-5 30 Figure 4.10 SEM image of CNT/MnO2NW-10 31 Figure 4.11 SEM image of CNT/MnO2NW-20 31 Figure 4.12 SEM image of CNT/MnO2NW-30 31 Figure 4.13 Cyclic voltammograms of MnO2NW printed at different times in 1mV/s 33 Figure 4.14 Cyclic voltammograms of 20 cycles of MnO2NW printed at different scan rates 33 Figure 4.15 Specific Capacitance Values of CNT/MnO2NW at different Scanning Rates for different Print Times 33 Figure 4.16 Constant Current Charge and Discharge Graphic of Pure CNT 37 Figure 4.17 Constant current charge and discharge pattern of CNT/MNO2NW5 37 Figure 4.18 Constant current charge and discharge pattern of CNT/MNO2NW10 37 Figure 4.19 Constant current charge and discharge pattern of CNT/MNO2NW-20 38 Figure 4.20 Constant current charge and discharge pattern of CNT/MNO2NW30 38 Figure 4.21 Constant current charge and discharge pattern at 0.25μA/cm2 38 viii Figure 4.22 Comparison of galvanostatic charge/discharge capacitance values at different current densities 39 Figure 4.23 Charge and discharge diagram of two series electrodes 40 Figure 4.24 Comparison with Single Electrode Charge and Discharge 41 Figure 4.25 Long-cycles stability 42 ix 4.5 CNT/MnO2NW-5, 10, 20, 30 cyclic voltammetry The capacitance effect caused by different printing times is discussed using cyclic voltammetry The voltage range is 0-0.8V, and the scan rate is 1, 2, 5, and 10 mV/s The first lap of the scan is observed The three-cycle volt-ampere graphs all have a similar rectangular shape, and the capacitance-to-capacitor values calculated by cyclic voltammetry are compared The capacitance data is summarized as shown in Figure 4.13 and Table 4.1 According to the results of the data, the specific capacitance value of the 20 printing times is the best At a scanning rate of mV/s, it can reach 431.25 μF/cm2; the number of printing times 5, and the capacitance value is the worst The capacitance value is 162.27μF/cm2, which may be due to the lower amount of manganese dioxide deposited, thereby affecting the performance of the capacitance effect; and when the number of printing times is 30, the specific capacitance value decreases with the increase in the number of MnO2, suggesting that the amount of MnO2 increases, MnO2 accumulates and the holes are covered, affecting the entry and exit of ions, the benefit of CNTs on the substrate to help conduct electricity is reduced, and the overall capacitance performance deteriorates, but it is printed 10 times and times In contrast, although the surface MnO2 is too dense, the quasi-capacitive nature of manganese dioxide is better than that of the carbon nanotubes Therefore, the specific capacitance value of 30 times printing is 190.63 μF/cm2, which is larger than the number of printing and 10 times results 32 Current(A) x -6 x -6 x -6 0 - x -6 - x -6 - x -6 - x -6 C C C C C N N N N N T T/ T/ T/ T/ M M M M 0 nO nO nO nO -5 -1 -2 -3 0 P o t e n tia l( V ) Current(A) Figure 4.13 Cyclic voltammograms of MnO2NW printed at different times in 1mV/s x -5 x -5 x -5 0 - x -5 - x -5 - x -5 m V /s m V /s m V /s m V /s 0 P o te n tia l( V ) Figure 4.14 Cyclic voltammograms of 20 cycles of MnO2NW printed at different scan rates Figure 4.15 Specific Capacitance Values of CNT/MnO2NW at different Scanning Rates for different Print Times 33 Table 4.1 Cyclic Voltammetry Capacitance Data for MnO2NW Modified CNTs of Different Orders Unit:μF/cm2 Scan rate(mV/s) 10 CNT 125.52 120.37 109.70 97.5 CNT/MnO2NW-5times 162.27 160.65 153.88 153.90 CNT/MnO2NW-10times 165.47 135.43 133.75 132.46 CNT/MnO2NW-20times 431.25 388.48 368.75 348.43 CNT/MnO2NW-30times 190.63 169.92 125.78 76.32 4.6 CNT/MnO2NW-20 Constant Current Charge and Discharge Cycle Test In the galvanostatic charge and discharge test, the current densities selected were 0.25, 0.625, 1.25, 2.5, 6.25, and 12.5 μA/cm2 It can be seen from Figures 4.16, 4.17, 4.18, 4.19, and 4.20 that the discharge process is not completely straight Considered as the voltage effect caused by the internal resistance, the result of the galvanostatic charge and discharge graph can calculate the IR drop, the internal resistance, the specific capacitance of the discharge, and the Coulomb efficiency The data can be used to discuss the effect of a capacitor, such as table, where IR drop, The internal resistance, specific capacitance of the discharge, and Coulomb efficiency are described as follows: - IR drop: During charge and discharge, the over-potential due to electrode polarization leads to a drop in the charge-discharge cut-off voltage This calculation method is the highest point potential of the initial discharge minus the second point potential 34 - Internal resistance: Where V is IR drop, I is to use the electric capacity, quantify the electrode polarization phenomenon - The specific capacitance of the discharge is: Where I is the current used, t is the discharge time, m is the electrode use area, and ∆V is the use potential range - Coulomb efficiency : This is the charge-discharge performance The change in conductivity, the influence of the structure, and the suitability of the electrolyte can be observed, and all of the above factors influence the value Next, the electrode obtained for four different printing times was subjected to a capacitive discussion From the measurement results, it can be seen that the capacitance values of electrodes with different printing times decreased with increasing capacitance density as shown in Table 4.2 The reason is that because of the low current density, electrolyte ions can easily enter the crystal lattice channel of manganese dioxide to carry out charge transfer, resulting in a significant increase in the specific capacitance value Conversely, at high current density, the specific capacitance value decreases This is because in the case of large current density, the electrolyte ions enter and exit very rapidly, and the electrode is easily polarized, so that the ions cannot diffuse deeply into the material and can only react on the surface, and if the working voltage cannot be loaded, the electrode is generated Increasing the current density also affects the Coulomb efficiency, because the ions only undergo adsorption and desorption on the surface, and no additional reaction occurs, so the Coulomb efficiency is high The discharge specific capacitance values of different printing times are compared as shown in Figure 4.22 When the number of printing times is 20, since the pores of the manganese dioxide are structurally intact, the charge transfer is good, so at 35 the low current density of 0.25 μA/cm2, the most The good specific capacitance value is 397.19μF/cm2, and when the number of prints is 30, the excess resistance of the manganese dioxide increases, resulting in a rise in the resistance of the electrode The capacitance thus exhibited decreases, and the specific capacitance value is 221.88 μF/cm2 On the other hand, when the number of prints was or 10, the number of deposited manganese dioxide was smaller, and the specific capacitance was also lower The specific capacitance values obtained were 163.75 and 189.38 μF/cm2 , respectively If the observation is performed with Coulomb efficiency data in Table 4.3, the electrode with a Coulomb efficiency of 78% ~ 87% can be printed 20 times, but at the same time the internal resistance is also the lowest; the number of prints is times The highest efficiency value is 92.09% The reason is that the reason is that the higher current value is used when printing five times When charge and discharge tests are performed, the charge is rapidly absorbed and desorbed on the surface of the material, and the side reactions are less than those of other printing parameters The highest Coulomb efficiency can be obtained The discharge specific capacitance and coulomb efficiency can be used to know whether ions or protons can enter the crystal lattice to perform charge transfer After synthesizing the two, the electrodes with 20 print times show the best effect The CNT/MnO2NW-20 electrode performs most prominently in cyclic voltammetry and galvanostatic charge and discharge, so the electrode will be used for a long period of galvanostatic charge and discharge tests to observe whether it has the characteristics of stability in a supercapacitor 36 µ F /c m µ F /c m 2 µ F /c m 2 µ F /c m Potential(V) 0 200 400 600 800 T im e ( s ) Figure 4.16 Constant Current Charge and Discharge Graphic of Pure CNT 2 µ F /c m µ F /c m 2 µ F /c m 2 µ F /c m Potential(V) 0 200 400 600 800 1000 1200 T im e (s ) Figure 4.17 Constant current charge and discharge pattern of CNT/MNO2NW-5 5 Potential(V) 0 200 400 600 800 1000 1200 1400 1600 1800 T im e ( s ) Figure 4.18 Constant current charge and discharge pattern of CNT/MNO2NW-10 37 5 Potential(V) 0 500 1000 1500 2000 2500 3000 T im e ( s ) Figure 4.19 Constant current charge and discharge pattern of CNT/MNO2NW-20 5 Potential(V) 0 200 400 600 800 1000 1200 1400 1600 T im e ( s ) Figure 4.20 Constant current charge and discharge pattern of CNT/MNO2NW-30 CNT C N T /M n O 2- C N T /M n O 2- C N T /M n O 2- Potential(V) C N T /M n O 2- 0 0 500 1000 1500 2000 2500 3000 T im e ( s ) Figure 4.21 Constant current charge and discharge pattern at 0.25μA/cm2 38 Discharge capacitance (µF/cm2) 400 P u re C N T C N T /M n O - C N T /M n O - C N T /M n O - C N T /M n O - 350 300 250 200 150 100 50 0 C u rre n t d e n s ity (µ A /c m ) Figure 4.22 Comparison of galvanostatic charge/discharge capacitance values at different current densities Table 4.2 MnO2 Modified CNT Constant Current Charge/Discharge Capacitance and Coulomb Efficiency Data for Different Times 0.25 μA/cm2 Charge (μF/cm2) Discharge (μF/cm2) Coulomb Efficiency(%) CNT 124.38 119.69 96.23 CNT/MnO2NW-5 177.81 163.75 92.09 CNT/MnO2NW-10 303.75 189.38 62.35 CNT/MnO2NW-20 507.50 397.19 78.26 CNT/MnO2NW-30 255.31 221.88 86.90 Table 4.3 Specific capacitance and coulombic efficiency data of CNT/MnO2NW-20 at different current densities CNT/MnO2NW-20 Charge (μF/cm2) Discharge (μF/cm2) Coulomb Efficiency(%) 0.25 μA/cm2 507.50 397.19 78.26 0.625 μA/cm2 350.78 307.03 87.53 1.25 μA/cm2 314.69 265.31 84.31 2.5 μA/cm2 312.50 256.25 82.00 39 4.7 Series Capacitor Charge and Discharge Test Since this experiment is a symmetric electrode system, its disadvantage is that the operating voltage is too small to be practical enough Therefore, we initially connect the two capacitive elements in series and amplify their operating voltages via galvanostatic charge and discharge tests, as shown in Figure 4.23 It can be seen that after the series connection, the charge-discharge pattern maintains a symmetric-like triangle, and its operating voltage can be successfully amplified from 0.8V of a single device to 1.6V, and the charge and discharge time of the series element is almost the same as that of a single element Figure 4.24 speculates that during the series assembly process of the entire component, there was no problem of poor interface contact, proving that this series capacitor component can improve the problem of too low operating voltage µ A /cm 2 µ A /cm 25 µ A /cm 2 µ A /cm Potential(V) 0 0 500 1000 50 2000 00 T im e (s) Figure 4.23 Charge and discharge diagram of two series electrodes 40 1.8 Series connection Single cell 1.6 Potential(V) 1.4 1.2 1.0 0.8 0.6 0.4 0.2 0.0 500 1000 1500 2000 2500 3000 Time(s) Figure 4.24 Comparison with Single Electrode Charge and Discharge 4.8 Comparison of Literature In this experiment, conductive ink and manganese dioxide ink were used by simple using a printer to spray onto commercially available paper to obtain a supercapacitor electrode In addition, the use of drugs is also relatively simple or harmless to the environment, or it is not necessary to produce in a special environment At present, manganese dioxide has not yet been configured as an ink for inkjet printing According to the literature comparison, the specific capacitance per unit area obtained in this experiment is not inferior to the specific capacitance value of other literatures Follow Table 4.4 below: 41 Table 4.4 Different Non-Contact Deposition Methods vs Capacitor Data for Solid state Superapacitors with Different Carbon Materials Material Method Electrolyte Areal specific capacitance (µF/cm2) Graphene Inkjet printed PVA/H3PO4 100 Graphene oxide Inkjet printed PVA/H2SO4 4.04 chelated graphene and (GQDs) Electrophoretic deposition PVA/H3PO4 9.09 VACNTs Laser-assisted dry transfer Ionic liquid gel 430 CNT/MnO2NW Inkjet printed PVA/LiCl 431.25 4.9 Long-cycles stability Figure 4.25 Long-cycles stability After using CNT/MnO2-20 to test the charge and discharge of 3000 cycles, the capacitor retention rate can be known after 3000 cycles Only a 35% capacitance retention can be maintained, presumably due to the solid state electrolyte curing causing ion transfer to be affected 42 PART CONCLUSION This experiment uses inkjet printing technology to deposit CNT and manganese dioxide on a photo paper for fabricating a solid state supercapacitor The electrochemical properties were measured Several conclusions are summarized here: CNT ink and MnO2 ink were produced to fabricate solid state supercapacitor electrodes through contactless deposition We used inkjet printing technology to deposit CNTs on photo paper to produce a conductive film of 500 Ω/sq., followed by depositing manganese dioxide on the conductive film to enhance its capacitive properties From cyclic voltammograms and galvanostatic charge-discharge diagrams, it can be seen that when the number of printed manganese dioxide reaches 20, the size of the tunnels is about 4.6 Å, which is just suitable for the diffusion of ions and the embedding/insertion of active materials The highest specific capacitance value of 397.19 μF/cm2 can be obtained at 0.25 μA/cm2 for the capacitor element The electrochemical properties of CNT/MnO2NW were significantly improved, and the most complete CNT/MnO2NW-20 capacitance value in the structure was 431 μF/cm2 , which is nearly 3.5 times as high as that of CNT with the capacitance value being 125 μF/cm2 The capacitor system adopts solid electrolyte This type of electrolyte is free from danger of liquid leakage, therefore the packaging cost will be reduced 43 REFERENCES R Bollström, A Määttänen, D Tobjưrk, P Ihalainen, N Kaihovirta, R.Ưsterbacka, J Peltonen, M Toivakka, A multilayer coated fiber-based substratesuitable for printed functionality, Organic Electronics 10 1020-1023, 2009 R Bollström, M Tuominen, A Määttänen, J Peltonen, M Toivakka, Top layer coatability on barrier coatings, Progress in Organic Coatings 73 26-32, 2012 R Bollström, J.J Saarinen, J Räty, M Toivakka, Measuring solvent barrier properties of paper, Measurement Science and Technology 23 015601, 2012 R Bollström, R Nyqvist, J Preston, P Salminen, M Toivakka, Barrier properties created by dispersion coating, Tappi Journal 12 (4) 45-51, 2013 R Bollström, D Tobjörk, P 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University of Agriculture and Forestry Degree Program Student name Studen ID Bachelor of Environmental Science and Management Nguyen Chi Cong DTN1454290005 FABRICATION OF SOLID STATE SUPERCAPACITORS. .. fabricate solid state supercapacitor electrodes through contactless deposition We used inkjet printing technology to deposit CNTs on photo paper to produce a conductive film of 500 Ω/sq., followed by. .. system adopts solid electrolyte This type of electrolyte is free from danger of liquid leakage, therefore the packaging cost will be reduced Key-words: Ink jet printing; Solid state supercapacitor;