臺灣博碩士論文加值系統

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Contents
中文摘要 i
Abstract iii
Contents v
Figure captions ix
Table list xvii
Chapter 1 Introduction 1
1.1 Research background 1
1.2 Cooling 2
1.3 Electrocaloric effect 3
1.4 Antiferroelectricity 6
1.5 Zirconium dioxide 7
1.6 Motivation of this study 10
1.7 Methodology 11
1.8 Dissertation organization 12
Chapter 2 Ti-doped ZrO2 antiferroelectric capacitors via HiPIMS system 22
2.1 Introduction 22
2.2 Experimental 27
2.2.1 Preparation of Ti-doped ZrO2 antiferroelectric capacitors 27
2.2.2 Characterization of materials and devices 28
2.3 Results and discussion 29
2.3.1 Material analyses of Ti-doped ZrO2 thin films 29
2.3.2 Electrical behaviors of Ti-doped ZrO2 antiferroelectric MIM capacitors 32
2.3.3 Electrocaloric effects of Ti-doped ZrO2 antiferroelectric MIM capacitors 35
2.4 Summary 37
Chapter 3 Highly reliable ZrO2 antiferroelectric capacitors with Al2O3 incorporation 58
3.1 Introduction 58
3.2 Experimental 61
3.2.1 Preparation of ZrO2 antiferroelectric capacitors with Al2O3 incorporation 61
3.2.2 Characterization of materials and devices 62
3.3 Results and discussion 64
3.3.1 Material analysis of ZrO2 thin films with Al2O3 incorporation 64
3.3.2 Electrical behaviors of ZrO2 antiferroelectric capacitors with Al2O3 incorporation 66
3.3.3 Electrocaloric effects of ZrO2 antiferroelectric capacitors with Al2O3 incorporation 69
3.4 Summary 71
Chapter 4 High-performance ZrO2 antiferroelectric capacitors with ZrN interfacial layer 86
4.1 Introduction 86
4.2 Experimental 88
4.2.1 Preparation of ZrO2 antiferroelectric capacitors with ZrN interfacial layer 88
4.2.2 Characterization of materials and devices 89
4.3 Results and discussion 89
4.3.1 Material analysis of ZrO2 antiferroelectric thin films with ZrN interfacial layer 89
4.3.2 Electrical behaviors of ZrO2 antiferroelectric capacitors with ZrN interfacial layer 91
4.3.3 Electrocaloric effect of ZrO2 antiferroelectric capacitors with ZrN interfacial layer 94
4.4 Summary 95
Fig. 4-4 GIXRD patterns of ZrO2 thin films with different cycles of ZrN layer. 99
Fig. 4-5 Grain size of ZrO2 thin films with different cycles of ZrN layer. 99
Fig. 4-6 HRTEM images of (a) w/o and (b) ZrN_9. 100
Fig. 4-7 (a) I-V and (b) P–E hysteresis loops of AFE ZrO2 MIM capacitors with different cycles of ZrN layer. 101
Fig. 4-8 The values of (a) ESD and (b) efficiency of all samples obtained from the P–E curves. 101
Fig. 4-9 Cycling endurance characteristics of efficiency of all samples. . 102
Fig. 4-10 Isw-t curves under different electric field of (a) w/o and (b) ZrN_9. 102
Fig. 4-11 Isw0 −Ea curves to extract RL and Ec of (a)w/o and (b) ZrN_9. 103
Fig. 4-12 The schematic of the MIM capacitors with (a) w/o and (b) ZrN_9 before and after the RTA process. 103
Fig. 4-13 P–E curves of (a) w/o, (b) ZrN_3, (c) ZrN_6, (d) ZrN_9, and (e) ZrN_12 at temperatures ranging from 298K to 388K. . 104
Fig. 4-14 P–T curves of the MIM capacitors. . 105
Fig. 4-15 ΔT of all samples under different temperature. 105
Fig. 4-16 ΔT of all samples under different numbers of cycling endurance tests. 106
Fig. 4-17 COP of all samples under different numbers of cycling endurance tests. 106
Chapter 5 ZrO2 ferroelectric capacitors with graphene top electrode 108
5.1 Introduction 108
5.2 Experimental 109
5.2.1 Preparation of ZrO2 capacitors with graphene top electrode and ZrN interfacial layer 109
5.2.3 Characterization of materials and devices 110
5.3 Results and discussion 111
5.3.1 Material analysis of ZrO2 thin films with graphene top electrode and ZrN interfacial layer 111
5.3.2 Electrical behaviors of ZrO2 capacitors with graphene top electrode and ZrN interfacial layer 112
5.3.3 Electrocaloric effect of ZrO2 antiferroelectric capacitors with graphene top electrode and ZrN interfacial layer 114
5.4 Summary 115
Chapter 6 Conclusion and future works 124
6.1 Conclusion 124
6.2 Future works 125
References 126
Publication list 150

 
Figure captions
Fig. 1 1 Technological evolution. 15
Fig. 1 2 Issue of heat accumulation in 3D structure [1.35]. 15
Fig. 1 3 48 yeas of microprocessor trend data [1.36]. 16
Fig. 1 4 The mechanism of electrocaloric effect [1.37]. 16
Fig. 1 5 The polarization domain in antiferroelectric material [1.38]. 17
Fig. 1 6 The definition of energy storage in dielectric capacitor [1.39]. 17
Fig. 1 7 Charge accumulated in dielectric capacitor with and w/o polarization [1.40]. 18
Fig. 1 8 Comparison of the energy storage in paraelectric, antiferroelectric, ferroelectric, and relaxor [1.41]. 18
Fig. 1 9 Phase diagram of ZrO2 under different temperature and pressure [1.26]. 19
Fig. 1 10 Polarization characteristics in variation ratio of HfxZr1-xO2 [1.42]. 19
Fig. 1 11 Polarization characteristics of ZrO2 with different capping layer [1.43]. 20
Fig. 1 12 XRD patterns of HfO2, Hf0.5Zr0.5O2, and ZrO2 [1.42]. 20
Fig. 1 13 Phase transition of the antiferroelectric ZrO2 thin film [1.42]. 21
Fig. 2 1 (a) Schematic diagram of co-sputtering in HiPIMS with pure Ti and Zr targets. The pulsed powers of Ti and Zr targets were 50 W and 80 W, respectively. (b) Co-sputtering timetable to open (on) and close (off) the Ti and Zr shutters for the incorporation of Ti in ZrO2 films. 39
Fig. 2 2 The structure of Ti-doped ZrO2 antiferroelectric capacitor. 40
Fig. 2 3 (a) O 1s XPS spectra and (b) XPS PARs and binding energy shift of non-lattice oxygen of ZrO2 thin films with various argon-to-oxygen ratios. 41
Fig. 2 4 (a) O 1s XPS spectra and (b) cumulative distribution of PARs of Zr-O bonds, Ti-O bonds and non-lattice oxygen of Ti-doped ZrO2 thin films with various percentages of Ti doping. 42
Fig. 2 5 Zr 3d XPS spectra, and of Ti-doped ZrO2 thin films with various percentages of Ti doping. 43
Fig. 2 6 SIMS depth profiles of Ti-doped ZrO2 thin films with various percentages of Ti doping. 44
Fig. 2 7 GIXRD patterns of ZrO2 thin films with various argon-to-oxygen ratios. 45
Fig. 2 8 GIXRD patterns of Ti-doped ZrO2 thin films with various percentages of Ti doping. 46
Fig. 2 9 HRTEM images of (a) ZrO2 thin films and (b) Ti-doped ZrO2 thin films. 47
Fig. 2 10 The definition of energy storage (ESD) and energy loss. 48
Fig. 2 11 (a) P–E curves of AFE ZrO2 MIM capacitors with various argon-to-oxygen ratios at the pulse width of 3 ms and (b) the efficiency extracted from the P-E curves at different pulse width. 48
Fig. 2 12 P–E curves of ZrO2, (a) Zr0.9Ti0.1O2, (b) Zr0.85Ti0.15O2, and (c) Zr0.8Ti0.2O2 MIM capacitors. 49
Fig. 2 13 The statistical distribution of (a) ESD and (b) efficiency of Ti-doped ZrO2 MIM capacitors with various percentages of Ti doping. 50
Fig. 2 14 Endurance behaviors of Ti-doped ZrO2 MIM capacitors with various percentages of Ti doping. 50
Fig. 2 15 P–E curves of (a) ZrO2, (b)Zr0.9Ti0.1O2, (c) Zr0.85Ti0.15O2, and (d) Zr0.8Ti0.2O2 MIM capacitors. before and after a 106-cycle endurance test. 51
Fig. 2 16 J–t curves of ZrO2 MIM capacitors with various percentages of Ti doping at (a) positive bias and (b) negative bias. 52
Fig. 2 17 The waveform of (a) positive bias and (b) negative bias applied in the measurement of J-t curves. 52
Fig. 2 18 J–t curves of (a) ZrO2, (b)Zr0.9Ti0.1O2, (c) Zr0.85Ti0.15O2, and (d) Zr0.8Ti0.2O2 MIM capacitors before and after a 106-cycle endurance test at positive bias. 53
Fig. 2 19 J–t curves of (a) ZrO2, (b)Zr0.9Ti0.1O2, (c) Zr0.85Ti0.15O2, and (d) Zr0.8Ti0.2O2 MIM capacitors before and after a 106-cycle endurance test at negative bias. 54
Fig. 2 20 P–E curves of (a) ZrO2, (c) Zr0.9Ti0.1O2, (e) Zr0.85Ti0.15O2, and (g) Zr0.8Ti0.2O2 MIM capacitors at temperatures ranging from 298K to 388K and (b), (d), (f), and (h) the P–T curves at various electric fields. 55
Fig. 2 21 CP–T curve of each ZrO2 thin film at various temperatures. 56
Fig. 2 22 P–T curves of (a) ZrO2, (b)Zr0.9Ti0.1O2, (c) Zr0.85Ti0.15O2, and (d) Zr0.8Ti0.2O2 MIM capacitors measured at an electric field of 4 MV/cm. 56
Fig. 2 23 ΔT of Ti-doped ZrO2 thin films as the function of temperature estimated from 298K to 388K. 57
Fig. 3 1 The structure of ZrO2 antiferroelectric capacitor with Al2O3 incorporation. 72
Fig. 3 2 GIXRD patterns of ZrO2 thin films with different Al2O3 incorporation percentages. 72
Fig. 3 3 XRR spectra of ZrO2 thin films with different Al2O3 incorporation percentages. 73
Fig. 3 4 HRTEM images of (a) ZrO2 and (b) 1% Al:ZrO2 thin films. 74
Fig. 3 5 UV–Vis optical transmission spectra of ZrO2 thin films with different Al2O3 incorporation percentages. 75
Fig. 3 6 (a) I–V curves and (b) P–E hysteresis loops of AFE ZrO2 MIM capacitors with different Al2O3 incorporation percentages. 76
Fig. 3 7 The statistical distribution of (a) ESD and (b) efficiency of all samples obtained from the P–E curves. 76
Fig. 3 8 (a) I–V curves and (b) P–E hysteresis loops of AFE ZrO2 MIM capacitors with different Al2O3 incorporation percentages at higher bias. 77
Fig. 3 9 ε–V curves of AFE ZrO2 MIM capacitors with different Al2O3 incorporation percentages at the measurement frequency of 10 kHz. 77
Fig. 3 10 The (a) permittivity and (b) dielectric loss (tanδ) of all samples as a function of frequency measured at zero bias. 78
Fig. 3 11 The leakage current of AFE ZrO2 MIM capacitors with different Al2O3 incorporation percentages. 78
Fig. 3 12 (a), (c), (d), and (g) P–E curves of the MIM capacitors with pure ZrO2 and1% Al:ZrO2 thin films stressed for different cycles and (b), (d), (f), and (h) the cycling endurance characteristics of ESD and efficiency. 79
Fig. 3 13 DC I–V curves of the MIM capacitors with (a)-(b) pure ZrO2 and (c)-(d) 1% Al:ZrO2 thin films stressed for different cycles at positive and negative bias. 80
Fig. 3 14 ln(J/E) versus 1/kT characteristics of (a)-(b) pure ZrO2 and (c)-(d) 1% Al:ZrO2 MIM capacitors before and after a cycling endurance test of 106 cycles. 81
Fig. 3 15 The activation energy versus the square root of the electric field characteristics of (a) ZrO2 and (b) 1% Al:ZrO2 MIM capacitors under different numbers of cycling endurance tests with positive and negative bias. 82
Fig. 3 16 Cycling endurance characteristics of the trapping levels of the defects within the pure ZrO2 and 1% Al:ZrO2 thin films under the (a) BE and (b) TE injections. 82
Fig. 3 17 The energy band diagrams of the MIM capacitors with (a) pure ZrO2 and (b) 1% Al:ZrO2 thin films under the BE injection. The samples with 1% Al:ZrO2 thin films can suppress the tunneling probability of the electrons through the ZrO2 thin film for fewer defects generated within the dielectric layer. 83
Fig. 3 18 P–E curves of the MIM capacitors with (a) pure ZrO2 and (b) 1% Al:ZrO2 thin films at temperatures ranging from 298K to 388K. 83
Fig. 3 19 P–T curves of the MIM capacitors with (a) pure ZrO2 and (b) 1% Al:ZrO2 thin films measured at an electric field of 3 and 4 MV/cm, respectively, under different numbers of cycling endurance tests. 84
Fig. 3 20 ΔT of the MIM capacitors with (a) pure ZrO2 and (b) 1% Al:ZrO2 thin films as the function of temperature estimated from 298K to 388K under different numbers of cycling endurance tests. 84
Fig. 4 1 The structure of ZrO2 antiferroelectric capacitor with ZrN interfacial layer. 97
Fig. 4 2 The atomic percentage of all the elements under different Ar sputtering time during XPS detection. 97
Fig. 4 3 (a) O 1s XPS spectra of ZrO2 thin films with different cycles of ZrN layer and (b) XPS PARs of Ti-O under different Ar sputtering times. 98
Fig. 4 4 HRTEM images of (a) w/o and (b) ZrN_9. 100
Fig. 4 5 (a) I-V and (b) P–E hysteresis loops of AFE ZrO2 MIM capacitors with different cycles of ZrN layer. 101
Fig. 4 6 Cycling endurance characteristics of efficiency of all samples. 102
Fig. 4 7 Isw-t curves under different electric field of (a) w/o and (b) ZrN_9. 102
Fig. 4 8 "Isw0" −Ea curves to extract RL and Ec of (a)w/o and (b) ZrN_9. 103
Fig. 4 9 The schematic of the MIM capacitors with (a) w/o and (b) ZrN_9 before and after the RTA process. 103
Fig. 4 10 P–E curves of (a) w/o, (b) ZrN_3, (c) ZrN_6, (d) ZrN_9, and (e) ZrN_12 at temperatures ranging from 298K to 388K. 104
Fig. 4 11 P–T curves of the MIM capacitors with w/o and ZrN_9. 105
Fig. 4 12 ΔT of all samples under different temperature. 105
Fig. 4 13 ΔT of all samples under different numbers of cycling endurance tests. 106
Fig. 4 14 COP of all samples under different numbers of cycling endurance tests. 106
Fig. 5 1 The structure of ZrO2 capacitor with graphene top electrode and ZrN interfacial layer. 116
Fig. 5 2 GIXRD patterns of ZrO2 capacitor with graphene top electrode and ZrN interfacial layer and TiN/ZrO2/TiN capacitor. 116
Fig. 5 3 The d-spacing of ZrO2 capacitor with graphene top electrode and ZrN interfacial layer extracted from XRD patterns. 117
Fig. 5 4 HRTEM images of (a) GZrN_0 and (b) GZrN_9. 118
Fig. 5 5 NBED of (a) GZrN_0, (b) GZrN_3, (c) GZrN_6, (d) GZrN_9, (e) GZrN_12 and (f) TiN/ZrO2/TiN capacitor. 119
Fig. 5 6 I-V and P-E curves of GZrN_9. 120
Fig. 5 7 PUND measurement of GZrN_9. 120
Fig. 5 8 (a) I-V and (b) P-E curves of ZrO2 capacitor with graphene top electrode and ZrN interfacial layer measured via PUND method. 121
Fig. 5 9 ε–V curves of ZrO2 capacitor with graphene top electrode and ZrN interfacial layer. 121
Fig. 5 10 P–E curves of (a) GZrN_0, (b) GZrN_3, (c) GZrN_6, (d) GZrN_9, (e) GZrN_12 measured via PUND method at temperatures ranging from 298K to 388K. 122
Fig. 5 11 P–T curves of ZrO2 capacitor with graphene top electrode and ZrN interfacial layer at temperatures ranging from 298K to 388K. 123
Fig. 5 12 ΔT of ZrO2 capacitor with graphene top electrode and ZrN interfacial layer at temperatures ranging from 298K to 388K. 123

 
Table list
Table 2 1 AFE and EC behaviors of Ti-doped ZrO2 thin films with various percentages of Ti doping. 57
Table 3 1 Benchmarks of the energy storage properties of this and other works. 85
Table 3 2 Benchmarks of electrocaloric effect of this and other works. 85
Table 4 1 Benchmarks of the energy storage properties of this and other works. 107
Table 4 2 Benchmarks of electrocaloric effect of this and other works. 107
 

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