設計具空間電荷特徵之金屬有機框架離子二極體薄膜來達成空前高效有機相滲透能源轉換

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研究生：	Amalia Rizki Fauziah Amalia Rizki Fauziah
論文名稱：	設計具空間電荷特徵之金屬有機框架離子二極體薄膜來達成空前高效有機相滲透能源轉換 Engineered Metal-Organic Framework-Based Ionic Diode Membranes with Space Charges for Unprecedented Osmotic Energy Conversion from Organic Solutions
指導教授：	葉禮賢 Li-Hsien Yeh
口試委員:	葉禮賢 Li-Hsien Yeh 郭紹偉 Shiao-Wei Kuo 吳嘉文 Chia-Wen Wu 王丞浩 Chen-Hao Wang
學位類別：	碩士 Master
系所名稱：	工程學院 - 化學工程系 Department of Chemical Engineering
論文出版年：	2021
畢業學年度：	109
語文別：	英文
論文頁數：	126
中文關鍵詞：	Ion transport 、Ion current rectification 、Ionic diode membrane 、Metal-organic framework 、Nanofluidics 、Salinity gradient power
外文關鍵詞：	Ion transport, Ion current rectification, Ionic diode membrane, Metal-organic framework, Nanofluidics, Salinity gradient power
相關次數：	點閱：305 下載：0
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Abstract
Unraveling and boosting lithium ion (Li+) transport in subnanoscale confined spaces is crucial to development of high performance lithium-ion batteries because metal-organic frameworks (MOFs), crystalline materials with ordered subnanoscale channel structures, are extensively used as artificial solid electrolyte interface layer to protect the anode from lithium dendrite deposition. Moreover, there have been growing interest in energy harvesting from a salinity gradient (or called osmotic energy conversion) from organic solutions, but the output performance is still limited and below the commercial benchmark value (5 W/m2). In this study, we report on two types of subnanoscale ionic diode membranes, including (i) zeolitic imidazole framework-8 (ZIF-8)/polystyrene sulfonate (PSS) and a highly ordered cylindrical alumina nanochannel (CAN) membrane (named as ZIF-8/PSS@CAN) and (ii) ZIF-8/PSS and a highly ordered branched alumina nanochannel (BAN) membrane (named as ZIF-8/PSS@BAN). Experimental results demonstrate that the ZIF-8/PSS membranes we fabricated are of large-scale, continuous, pinhole-free and subnanoscale window-cavity structures and the PSS is of highly space-charged properties, so that the membranes can be used as a highly ion selective layer. Moreover, the two membranes are shown to exhibit significant diode-like ion current rectification effect, capable of amplifying ion transport at subnanoscale confinements. We therefore probe application of the two types of subnanoscale ionic diode membranes in osmotic energy conversion from organic solutions. We show that at a 50-fold LiCl concentration gradient in methanol, the ZIF-8/PSS@CAN can achieve a power density of 5.28 W/m2 and the output performance can be upgraded to an unprecedented value of 9.58 W/m2 by increasing the geometry gradient with using the ZIF-8/PSS@BAN. Note that the two values reported outperform all the previously reported ones. Realizing the ultrafast dehydrated ion transport in the subnanoscale confined spaces created by the MOF membranes we developed opens up valuable insights into not only exploiting next-generation high efficiency Li-ion batteries but also energy harvesting from salinity gradients in waste organic solutions. This path will likely ignite the way not only to help alleviate the environmental burden but also provide new energy resources for meeting the need of the ever-growing energy demand.

Table of Content

ABSTRACT    II
TABLE OF CONTENT    III
LIST OF FIGURES    V
LIST OF TABLES    XV
CHAPTER 1 INTRODUCTION    1
1.1.    Preface    1
1.2.    Motivation    2
1.3.    Literature review    4
1.4.    Objectives    12
CHAPTER 2 PRINCIPLES AND MECHANISMS    14
2.1.    Metal-organic framework    14
2.2.    Electric double layer    16
2.3.    Ion selectivity    18
2.4.    Ionic current rectification    19
2.5.    Osmotic energy conversion    22
CHAPTER 3 RESEARCH METHODS    28
3.1.    Chemicals and equipment    28
3.1.1.    Chemicals    28
3.1.2.    Equipment    29
3.1.3.    Analytical instruments    31
3.2.    Experimental section    34
3.2.1.    Fabrication process of the heterogeneous membrane fabrication process    34
3.2.2.    Performance test (electrical measurement) of the heterogeneous membrane    39
CHAPTER 4 RESULTS AND DISCUSSION    42
4.1.    Material characterization    42
4.1.1.    Scanning electron microscopy (SEM)    42
4.1.2.    N2 sorption isotherm    48
4.1.3.    X-ray diffraction (XRD)    49
4.1.4.    Fourier transform infrared spectroscopy (FTIR)    50
4.1.5.    Zeta potential    52
4.1.6.    Contact angle    52
4.2.    Ion transport properties    53
4.3.    Ion selectivity    64
4.4.    Osmotic energy generation performance    66
4.4.1.    Preferential direction    68
4.4.2.    Diffusion potential and diffusion current    70
4.4.3.    Maximum power density    72
4.5.    Stability test    87
4.5.1.    Material stability    87
4.5.2.    Ion transport stability    90
4.5.3.    Osmotic power generation stability    90
CHAPTER 5 CONCLUSION    28
CHAPTER 6 FUTURE PROSPECT    94
REFERENCES    95


 
List of Figures
Figure 1.1 Energy storage and conversion devices play a crucial role in the development of sustainable energy.    2
Figure 1.2 The schematic illustration diagram of the copper foil anode without (upper panel) and with (lower panel) coating a thin MOF membrane. The MOF-coated Cu foil indicating excellent stability of SEI layer. Hence, suppresses the formation of lithium dendrite.7    4
Figure 1.3 MOF-membrane-based osmotic power generation series with heterogeneous continuous subnanochannels.24-27    8
Figure 1.4 The generated maximum power density of various MOF-based membranes.24-27 The results show that the harvested osmotic power is considerably low and way below the commercial benchmark of 5 W/m2.    9
Figure 1.5 The salinity gradient energy generated from an organic solution system.28    11
Figure 1.6 Design of the heterogeneous continuous subnanocahnnel membrane. It consists of an ion selective layer of ZIF-8/PSSx and a support layer of ANM.    12
Figure 1.7 The schematic illustration of lithium-ion transport inside the cage of ZIF-8/PSSx.    13
Figure 2.1 Highly adjustable properties of MOFs. MOFs can be easily scaled, processed, and functionalized to render the new both physical and chemical properties for specific applications……………………………………………..…………….14
Figure 2.2 ZIF-8 crystalline structure. The SOD topology of ZIF-8, comprising of Zn(NO3)26H2O as the metal source and C4H6N2 as the organic linker, contains an angstrom-sized window of ~0.34 nm and a nanometer sized cavity of ~1.16 nm.    15
Figure 2.3 Simplified schematic illustration of the ion distribution for an electric double layer.    16
Figure 2.4 The Debye length as a function of electrolyte concentration. (a) EDL is not overlapping at a high concentration of electrolyte; thus, the distribution of cation and anion inside nanochannel is almost the same. (b) EDL is overlapping at a low concentration of electrolyte; thus there are more counterions (cations) adsorbed to the surface of the nanochannel.    17
Figure 2.5 Dependence of the charged nanochannel size on Debye length. (a) Weak ion selectivity occurs when the nanochannel radius (R) is longer than the Debye length; hence the EDL overlap is not obvious. On the other hand, (b) strong ion selectivity happens when the nanochannel radius is comparable to the Debye length; thus, the EDL overlap is obvious.    18
Figure 2.6 Schematic illustration of ion transport property in a symmetric nanochannel membrane system, with a linear I-V curve, indicating Ohmic behavior.    20
Figure 2.7 Schematic illustration of ion transport property in a nanochannel membrane system with asymmetric geometry and asymmetric charge distribution, showing an I-V curve with ICR and indicating the diode-like behavior.    21
Figure 2.8 Setup of Osmotic energy conversion device. The ion-selective membrane is put in the middle between two reservoirs which are filled with a high salt concentration in one side and a low salt concentration in another side. This whole process will output the diffusion potential and diffusion current.    24
Figure 2.9 Contributions of different resistances in the electrical measurement system of a salinity gradient energy conversion device. (a) Equivalent circuit diagram showing the various parts contribution to the overall measured current and voltage. (b) The obtained I-V curves in the presence of a concentration gradient. The measured VOC is composed of two parts: Vred and Vdiff. The osmotic contribution can be obtained by subtracting the Vred value.    26
Figure 2.10 Dependence of the applied external resistance on the osmotic power generation. (a) Generated current density, and (b) generated power density.    27
Figure 3.1 Cylindrical alumina nanochannel (CAN) membrane. CAN was fabricated in acidic environment using a modified two steps anodization as previously reported……………………………………………………………………..….37
Figure 3.2 Branched alumina nanochannel (BAN) membrane. BAN was fabricated in acidic environment using three steps anodization. The last step anodization was used to grow branched structure.    37
Figure 3.3 ZIF-8/PSSx@ANM was fabricated using solid confinement conversion method. ZIF-8/PSSx can be easily be grown on CAN and BAN.    38
Figure 3.4 The device set-up of ion transport properties test. Symmetric concentration of electrolyte is filled in the both of custom-made conductive reservoirs.    40
Figure 3.5 The device setup of osmotic energy conversions test. Both of custom-made conductive reservoirs are filled with different electrolyte concentrations, hence, there is an electrolyte concentration ratio applied.    40
Figure 4.1 The morphological structure and chemical composition of ZHN/PSSx@CAN. The SEM image of (a) cross section view (insets: showing higher magnification) and (b) top view of ZHN/PSS0@CAN. While, (c) top view of ZHN/PSS9@CAN. The EDX analysis of (d) ZHN/PSS0, and (e) ZHN/PSS9. There is S element that can be detected in the top view of ZHN/PSS9………………………………......42
Figure 4.2 The morphological structure observed from the cross section, top, and bottom view of as-prepared heterogeneous membrane of ZIF-8/PSS9@CAN. The SEM images clearly emphasize that continuous defect-free heterogeneous subnanochannel membrane was successfully fabricated.    43
Figure 4.3 The elemental mapping of ZIF-8/PSS9@CAN from the top view SEM image. The two main elements of Zn and S were detected, and the signal of the S element indicates that the PSS chain was successfully trapped inside ZIF-8 cage.    45
Figure 4.4 The cross-section, top, and bottom view SEM inages of ZIF-8/PSS9@BAN were examined to unveil their morphology. The SEM results clearly define that continuous crack-free subnanochannel ZIF-8/PSS9 can be grown on various kinds of substrates regardless the structure of the substrate itself.    46
Figure 4.5 The elemental mapping of ZIF-8/PSS9@BAN from of the top view SEM image, showing a similar result with the one@CAN. The same conclusion that intercalation of the PSS chains inside the ZIF-8 crystal still can be obtained even after changing different structures of the substrate.    47
Figure 4.6 SEM images of ZIF-8/PSSx in large scale with various PSS content. The crystalline structure of continuous crack-free ZIF-8/PSSx remains unchanged, revealing that it is independent of the amount of PSS content added.    48
Figure 4.7 Nitrogen sorption isotherms at 77 K of ZIF-8/PSSx with different PSS content. (a) The specific surface area of the ZIF-8/PSSx can be estimated by using the absorption-desorption curve and calculated according to the BET method; meanwhile, the pore size distributions of (b) ZIF-8/PSS9 and (c) ZIF-8/PSS14 were calculated based on N2 sorption isotherms estimated by GCMC (grand canonical Monte Carlo) method.    49
Figure 4.8 The XRD profiles of the heterogeneous continuous subnanochannel membranes at ZIF-8/PSSx and ANM sides. (a) There is no shift in the peak positions of ZIF-8/PSSx compared with those from ZIF-8 database. (b) The XRD profile of the substrate of ANM side indicates a single strong peak position at 45.2o.    50
Figure 4.9 FTIR spectra of ZIF-8/PSSx membranes. A distinctive absorption band shown in yellow region, associated with the existence of sulfonate group on PSS chains can be only observed for ZIF-8/PSS9.    51
Figure 4.10 The zeta potential of ZIF-8/PSSx. The charge of the membrane can be easily tuned by the content of PSS. ZIF-8/PSSx is more negatively charged upon the increase of PSS content.    52
Figure 4.11 The water contact angle measurement of themembrane at ZIF-8/PSSx side and ANM side. The results indicate that both sides of the membrane possess different wettability.    53
Figure 4.12 The ionic diode-like behavior of the heterogeneous continuous subnanochannel membrane of ZIF-8/PSSx@CAN under the symmetric concentration of electrolyte. (a) The scanned I-V curve of the as-prepared ZIF-8/PSSx@CAN under the symmetric concentration of electrolyte in 1 mM LiCl-methanol solution. The transmembrane ionic accumulation of ZIF-8/PSSx is more obvious along with the increase of PSS content. (b) The ICR ratio of the as-synthesized ZIF-8/PSSx@CAN is stepping up as the PSS loading content is getting higher.    55
Figure 4.13 The schematic illustration of the heterogeneous continuous subnanochannel membrane of ZIF-8/PSSx@CAN. The heterogeneous membrane possesses multiple asymmetries of pore sizes, charges, and wettability which further have significant advantages for amplifying the transmembrane current.    58
Figure 4.14 The investigation of ion transport properties of ZIF-8/PSSx with different structures of substrate (a) I-V curves of ZIF-8/PSSx@BANs with different PSS content under symmetric electrolyte concentration in methanol. (b) The ICR ratios of the ZIF-8/PSSx@CAN and ZIF-8/PSSx@BAN with various PSS content.    60
Figure 4.15 The schematic of more complex asymmetric pore sizes of the ZIF-8/PSSx@BAN, leading to the stronger asymmetric EDL overlapping degree and the higher ICR ratio.    61
Figure 4.16 The conductance recorded in symmetric electrolyte as a function of concentration of electrolyte using (a) ZIF-8/PSSx@CAN and (b) ZIF-8/PSSx@BAN.    63
Figure 4.17 I-V curves of the heterogeneous membrane under two configurations with different concentration gradient directions: (Olive green data) The 50 mM (high concentration) LiCl-methanol solution contacts with the ZIF-8/PSSx side, and the 10 symboM (low concentration) one contacts with the ANM side; (Dark green data) The 50 mM (high concentration) LiCl-methanol solution contacts with the ANM side, and the 10 M (low concentration) one contacts with the ZIF-8/PSSx side.    64
Figure 4.18 The schematic of osmotic energy conversion process. Under the concentration gradient between the as-prepared ZIF-8/PSSx@CAN membrane, the counterions (Li+) would always migrate from the high concentration region to the low concentration region naturally.    67
Figure 4.19 I-V curves of the ZIF-8/PSS9@CANs under two different configurations with forward and backward concentration gradients in LiCl-methanol system. The short circuit current (ISC) and open circuit voltage (VOC) can be obtained by the intercepts on y-axis and x-axis, respectively.    68
Figure 4.20 The I-V curves of the ZIF-8/PSS9@CAN under the forward LiCl concentration gradient in methanol before (dark red) and after (light red) the subtraction of Vred. The obtained open-circuit voltage (VOC) consists of two parts: redox potential (Vred) and diffusion potential (Vdiff). The pure Vdiff can be obtained by deducting the contribution of the Vred. The value of Vred was thoroughly evaluated experimentally without the existence of the ion selective membrane. Thus, the obtained voltage is fully contributed by the electrochemical redox reaction at the electrode surface.    70
Figure 4.21 The diffusion current density and diffusion potential of ZIF-8/PSS9@CAN as functions of the electrolyte concentration ratio in the LiCl-methanol environment. Both of Vdiff and Jdiff elevate proportionally along with the increasing concentration ratio.    72
Figure 4.22 The PSS content effect on the (a) current density and (b) power density of ZIF-8/PSSx@CAN as a function of external resistance in the methanol system.    73
Figure 4.23 Schematic illustration of the enhancement of Li+ transport in the nanoconfined space of ZIF-8 upon increasing the dosage of polyelectrolyte of PSS.    74
Figure 4.24 The PSS content effect on the (a) current density and (b) power density of ZIF-8/PSSx@BAN as a function of external resistance in the methanol system.    74
Figure 4.25 The osmotic energy conversion performance of the membrane in 50-fold LiCl-Methanol solution. (a) The generated current and power density of the homogenous membrane of CAN as a function of external load resistance. The current density is declining along the increasing of external resistance, while the power density reaches the maximum value in the moderate external resistance. (b) The extracted maximum power density value of homogenous membranes is always lower than the heterogeneous membrane. It goes up along with increasing the amount of loaded PSS in the ZIF-8 crystal.    75
Figure 4.26 The heterogeneous membrane design of ZIF-8/PSSx@CAN renders numerous advantages in the salinity gradient energy conversion process. It has a highly ion-selective layer stemming from the negatively charged tiny channel of ZIF-8/PSSx. More than that, ZIF-8/PSSx@CAN behaves like an ionic diode and contains a highly abundant order channel both from subnanochannel ZIF-8/PSSx and CAN which further can amplify the generated current. These effects simultaneously collaborate providing high generated osmotic power density.    77
Figure 4.27 The measured current and power density across ZIF-8/PSS9@CAN membrane in organic and aqueous solutions. The generated current and power density of ZIF-8/PSS9@CAN significantly enhance as organic solvent is used to dissolve the electrolyte.    78
Figure 4.28 Schematic of the size-exclusion of the hydrated Li+using the membrane with subnanometer ZIF-8/PSSx channels. Most of the ions are presented in the dehydrated state when the organic solvent of methanol is used as the solvent in which dehydrated ion size is substantially smaller than the window size of ZIF-8/PSSx. Therefore, the dehydrated ion can diffuse along the ZIF-8/PSS9@CAN membrane easily to generate high power density. On the other hand, the ion is presented in the hydrated state with larger ion size when the electrolyte is dissolved in water, hence, leading to low harnessed power density.    79
Figure 4.29 ZIF-8/PSS9@CAN was utilized to harvest osmotic energy from different LiCl salinity gradients (10-fold, 50-fold, and 100-fold) of the organic solution of methanol. (a) current density and (b) power density with the respect to the ionic concentration.    81
Figure 4.30 ZIF-8/PSS9@BAN was utilized to harvest osmotic energy from different LiCl salinity gradients (10-fold, 50-fold, and 100-fold) of the organic solution of methanol. (a) current density, and (b) power density with the respect to the ionic concentration.    82
Figure 4.31 Osmotic Energy Harvating Performance of the ZIF-8/PSSx@CAN and the ZIF-8/PSSx@BAN under various LiCl-methanol concentration gradients: (a) produced short circuit current and (b) measured power density.    83
Figure 4.32 Schematic of the effect of the pore size gradient on the osmotic energy generation performance. The enhancement of the generated short circuit current in the ZIF-8/PSSx@BAN is on account of the ion diffusion direction starting from the smallest channel of angstrom-scale to the moderate channel size of nano-channel to the biggest channel size of submicro-scale which finally causing the augmented electrostatic force.    84
Figure 4.33 Comparison of the maximum output of harnessed power density with heterogeneous membranes that have been reported before under 50-fold salinity gradients.     85
Figure 4.34 Comparison of the osmotic power generation performance of ZIF-8/PSS14@BAN along with different effective testing area. a) Output current density, and b) output power density versus external resistance.    86
Figure 4.35 (a) Cross-sectional and (b) top view SEM image of    87
Figure 4.36 Cross-sectional SEM images of the ZIF-8/PSS14@BAN and the corresponding elemental mapping images with EDX.  The ZIF-8/PSS14@BAN stays the same after soaking the membrane in the 500 Mm LiCl-methanol for 3 consecutive days. The elemental mapping demonstrates that S element still can be observed.    88
Figure 4.37 The XRD profiles of ZIF-8/PSS14 and ZIF-8/PSS0 on ANMs. The crystallinity of ZIF-8/PSS14 remain in good-agreement with ZIF-8 database. There is no shift in the peak position of ZIF-8/PSS14 after soaking in 500 mM LiCl methanol solution for 3 days in a row.    89
Figure 4.38 The conductance of ZIF-8/PSS9@BAN recorded for a long period of 72 h in a 100 mM solution of LiCl dissolved in methanol. The attained conductance keeps almost constant with only a small fluctuation during the test time of 72 h.    90
Figure 4.39 The measured short circuit currents of ZIF-8/PSS14@BAN continuously examined for a long period of 72 h in a 100 mM solution of LiCl dissolved in methanol. The current keeps almost constant within 72 h, proving that the heterogeneous membrane of ZIF-8/PSS14@BAN is high-persistent for generating osmotic energy and suitable for long-term operation continually.    91


 
List of Tables
Table 1.1 The osmotic power generation of the bio-inspired solid-state heterogeneous membranes under a 500 mM/10 mM electrolyte ratio.    6
Table 1.2 The osmotic power generation of the heterogeneous metal-organic framework-based membrane with subnano-scale channels.    10
Table 1.3 The osmotic power generation capability of the bio-inspired solid-state heterogeneous membrane in organic solvent.    11
Table 3.1 The chemicals used in alumina nanochannel membrane fabrication process…...28
Table 3.2 The list of chemicals utilized in the ZIF-8/PSSx thin membrane fabrication process………………………………………………………………………..29
Table 3.3 The chemicals employed in the electrical measurement test.    29
Table 4.1 The corresponding VOC, Vred, and Vdiff of ZIF-8/PSS9@CAN as a function of the concentration gradient………………………………………………………...71
Table 4.2 The maximum power density in 1000 Mm/ 1 mM LiCl-Methanol compared with recent research.    86

                                

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