高積集度非揮發性鐵電記憶體應用之含氧白金電極之研究

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研究生：	黃俊凱 Chun-Kai Huang
論文名稱：	高積集度非揮發性鐵電記憶體應用之含氧白金電極之研究 Integration and Electrical Characteristics of Ferrolectric Capacitors by Using PtOx Electrodes for High-density Embedded Nonvolatile Memory Application
指導教授：	吳泰伯 Tai-Bor Wu
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2005
畢業學年度：	93
語文別：	英文
論文頁數：	183
中文關鍵詞：	鐵電薄膜、非揮發性記憶體、含氧白金
外文關鍵詞：	ferroelectric, PZT, FeRAM, PtO
相關次數：	點閱：2 下載：0
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鐵電記憶體元件整合隨CMOS製程縮微，其電容由傳統平面發展為堆疊立體結構，製程當中面臨蝕刻與還原氣氛(forming gas)引起電性失效的問題。本研究探討適用高積集度記憶體元件之電極開發，提出含氧白金（PtOx）材料作為過渡模板的白金電極，解決傳統白金(Pt)電極不易蝕刻，側壁殘留於元件縮微時無法整合的問題，完成金屬-鐵電薄膜-金屬(MIM)堆疊電容結構整合。PtOx電極對於鋯鈦酸鉛（PZT）鐵電薄膜，其活性氧於熱處理中釋放，填補PZT與電極介面間的氧空缺，並使PZT薄膜受一壓應力，相較於Pt電極，提高殘留極化量與增加電性可靠度。在蝕刻PtOx電極中，藉由氧氣氛添加，其側壁氧化形成保護作用，可藉此得到高蝕刻選擇比，無殘留、側壁斜角大於75度的鐵電電容陣列。藉由控制PtOx電極中氧成份與功函數的提升，延滯Pt催化造成鐵電電容劣化，其漏電流機制蕭特基發射(Schotty emission)，介面缺陷與Schotty能障相關。最後，利用電子束微影製程與原子力顯微鏡檢測，完成90奈米尺度鐵電電容電性直接測量技術，其電容於90奈米尺度下仍維持高殘留極化量，並探討鐵電電容尺寸效應(size effect)，於80K低溫下，仍維持極化值。其研究成果可具體提供量產製造與標準檢驗流程供奈米級高密度非揮發性記憶體製程於次世代使用。

《Contents》

Table captions……………………………………………………….Ⅴ
Figure captions……………………………………………………...Ⅵ
Chapter 1    Introduction
1-1. Technology developments of ferroelectric memories………1
1-2. Motivation of the research…………………………………...4
1-3. Objectives of This Research………………………………….7

Chapter 2    Literature review
2-1. Ferroelectric materials………………………………………..11
2-2. Electrode materials for ferroelectric capacitors…………….13
2-3. Ferroelectric memories……………………………………….15
2-3-1. FERAM cell and operation……………………………16
2-3-2. Deposition techniques of ferroelectric capacitors…….18
2-3-3. Dry etching technologies of ferroelectric memories….19
2-3-4.Scaling…………………………………………………...21
2-4. Reliability issues of ferroelectric memories…………………23
2-4-1. General aspects…………………………………………23
2-4-2. Fatigue…………………………………………………..25
2-4-3. Retention………………………………………………..26
2-4-4. Imprint………………………………………………….27

Chapter 3    Enhancement in reliability characteristics of Pb(Zr0.4Ti0.6)O3 thin film capacitors by using PtOx electrodes
3-1. Introduction…………………………………………………...37
3-2. Experimental procedures……………………………………. 38
3-3. Results and Discussion………………………………………..39
3-4. Conclusion……………………………………………………..48

Chapter 4    Dry etching of submicron feature-size PZT    capacitors with PtOx top electrode for memory application
4-1. Introduction…………………………………………………...65
4-2. Experimental procedures……………………………………..67
4-2-1. Thin film deposition……………………………………67
4-2-2. Dry etching techniques………………………………... 67
4-3. Results and Discussion………………………………………..70
4-3-1. Etching characteristics of PtOx films………………….70
4-3-2. Etching characteristics of PtOx /PZT films capacitor stacks…………………………………………………...73
4-4. Conclusion……………………………………………………. 78

Chapter 5    Improvements in electrical properties of hydrogen-treated ferroelectric capacitors with PtOx top electrode for memory applications
5-1. Introduction…………………………………………………...98
5-2 Experimental procedures……………………………………...99
5-2-1 Thin films preparation and ferroelectric capacitors fabrication…………………………………………….100
5-2-2. Forming gas annealing………………………………...100
5-3. Results and Discussion……………………………………….101
5-3-1. RBS spectra analysis for the composition of deposited films……………………………………………………101

5-3-2. Characteristics of hydrogen-treated ferroelectric capacitors……………………………………………………...101
5-3-3. The relationship of the Schottky barrier height with defect concentrations…………………………………………109
5-4. Conclusion…………………………………………………….112

Chapter 6    Fabrication and electrical characterization of nanoscale PtOx/PZT/PtOx capacitors for G-bit embedded ferroelectric memory application
6-1. Introduction…………………………………………………..133
6-2. Experimental procedure and technique…………………….135
6-2-1. Thin film preparation…………………………………135
6-2-2. PtOx/PZT/PtOx/Pt capacitor fabrication…………….136
6-2-3. Measurement setup……………………………………137
6-3. Results and Discussion……………………………………….138
6-3-1. Structural characterization…………………………...138
6-3-2. Properties of PtOx/PZT/PtOx/Pt capacitor…………..138
6-3-3. Ferroelectric characteristics in nanoscale…………...141
6-4. Conclusion…………………………………………………….142

Chapter 7    Conclusions……………………………………………158

Reference…………………………………………………………….160















《Table captions》


Table 1-1    The technology development of FeRAM.                         9
Table 1-2    Nonvolatile Semiconductor Memory Market Estimates (in $Billion).  9
Table 2-1     Prospect of several integrated ferroelectric devices.               29
Table 3-1     Process parameters for PtOx and PZT films.                     49
Table 3-2    The elastic modulus and Poisson ratio for the materials.           50
Table 4-1    Etching recipes of PtOx and Pt films.                           79
Table 4-2    Etching recipes of PZT films.                                 79
Table 4-3    Ashing recipes of PR.                                        80
Table 5-1    The PtOx  and PZT composition of RBS spectra for scattering     2MeV He2+ ions from different PtO/PZT, PtO0.4/PZT and Pt/PZT configurations annealing at200℃ for 30min.                   114
Table 5-2    Parameters used in evaluating barrier height of top electrode/PZT capacitors.                                                115

《Figure Captions》


Figure 1-1    Integrated bluetooth single chip.                              10
Figure 1-2    Structure of Next-Generation Smart Card.                     10
Figure 2-1    ABO3 perovskite unit cell.                                   30
Figure 2-2    Hysteresis loop of a ferroelectric material.                      31
Figure 2-3    PbTiO3-PbZrO3 subsolidus phase diagram.                     32
Figure 2-4    (a) A 1T/1C memory cell. The cell consists of one transistor and one ferroelectric capacitor. (b)A 2T/2C memory cell.            33
Figure 2-5    Schematic diagram of Virtual Ground hysteresis measurement method.                                                  34
Figure 2-6    Effect of fatigue, imprint, and loss of retention of 1T/1C cells.     35
Figure 2-7    Schematic drawing of a sequential pulse for (a) fatigue (b) retention and (c) imprint measurement.                                36
Figure 3-1      (a) Resistivity of PtOx films as a function of O2 gas flow ratio and (b) the XRD pattern of PtOx films prepared with different Ar/O2 gas mixture ratio.                                              51
Figure 3-2      SEM micrographs of various PtOx films prepared under (a) Ar/O2 = 100/0, (b) Ar/O2 = 90/10, (c) Ar/O2 = 70/30, and (d) Ar/O2 = 50/50, respectively.                                               52
Figure 3-3      Surface morphology of PtOx film prepared with Ar/O2=70/30 gas mixture ratio (a) before RTA treated. (b) after RTA treatred at 600℃ in O2 ambient for 5min, the surface roughness from 3.41nm to 3.52nm after annealing.                                     54
Figure 3-4      XRD spectrums of PZT films deposited on the various PtOx and Pt electrode, followed by RTA treatment at 600℃in O2 ambient for 5min.
55
Figure 3-5      (a) P-E hystersis loops of PZT capacitors with various PtOx electrodes. (b) Pr and Ec value dependences of PZT capacitors obtained at various applied voltage.                                     56
Figure 3-6      The room temperature stress of PtOx thin films varied with different Ar/O2 gas mixture.                                         57
Figure 3-7      Room temperature stress state comparison of Pt and PtOx films with 600℃ RTA treatment for 5min as a function of deposition temperature.                                              58
Figure 3-8      XRD spectrums of PtOx films deposited at (a) 400℃ (b) 150℃, followed by RTA treatment at 600℃ in O2 ambient for 5min. (c) Pure Pt films for reference.                                       59
Figure 3-9      X-ray photoelectron spectra of Pt4f electrons for PtOx films deposited at (a) 400℃ (b) 150℃, followed by RTA treatment at 600℃ in O2 ambient for 5min.                                          60
Figure 3-10      Pulse-width dependence of polarization for PZT capacitors with different electrodes measured by 5V at room temperature.        61
Figure 3-11      Fatigue endurance behavior of different PZT capacitors structure with different electrodes under 5V bipolar cycles at a frequency of 1MHz.                                                    62
Figure 3-12      The retention properties of PZT capacitors structure with different electrodes configuration under 5ms pulse width ±5V read and write pulses at room temperature.                         63
Figure 3-13      Plot of the logarithm of switching polarization as a function of time with a stretched exponential function.                              64
Figure 4-1      Schematic diagram of the helicon wave plasma etch system.       81
Figure 4-2      Variation of etchng rate of PtOx and Pt films as a function of (a) source power(Etching fixed condition: bias power 250W, gas flow rate:40sccm, gas ratio: Ar/(20％)Cl2 and pressure: 5mTorr). (b) bias power (Etching fixed condition: source power 2100W, gas flow rate: 40sccm, gas ratio: Ar/(20％)Cl2 and pressure: 5mTorr), and (c) gas pressure (Etching fixed condition: source power2100W, bias power 250W, gas flow rate: 40sccm, and gas ratio: Ar/(20％) Cl2.        82
Figure 4-3      SEM micrograph of (a) Pt pattern and (b) PtOx pattern. Less sidewall residues are observed in PtOx pattern while etched in Ar/(20％)Cl2 gas mixture.(Etching condition, source power: 2100W, bias power: 250W gas pressure: 5mTorr and gas flow rate:40sccm.)           84
Figure 4-4      X-ray photoelectron spectra of Cl2p and Pt4f electrons from etched films: (a) Pt etched in Ar/Cl2(20％) (b) PtOx etched in Ar/Cl2(20％). 85
Figure 4-5      Etch rates of PtOx and Pt and their etching selectivity against photoresist (PR) as a function of O2 content in the Ar/Cl2/O2 plasma. (Etching condition: source power: 2100W, bias power 250W, gas pressure: 5 mTorr, and gas flow rate: 40sccm.)                  86
Figure 4-6      SEM micrograph of the PtO patterns etched in the Ar/(10％)O2/(20％)Cl2 plasma, after PR ashing , the etch slope was over 75°and free of residue. (a) Line pattern (b) Island pattern.                     87
Figure 4-7      X-ray photoelectron spectra of Pt4f electrons from etched films:(a) PtOx etched in Ar/Cl2(20％) (b) PtOx etched in Ar/Cl2 (20％)/O2(5％) plasmas. (c) PtOx etched in Ar/Cl2(20％) /O2(10％) plasmas, and (d) compared of Cl2p peak intensity with or without O2 addition in etching gas mixture.                                        88
Figure 4-8      Etch rates of PtOx and PZT and their etching selectivity as a function of Cl2 content in the Ar/(10％)O2/Cl2 plasma. (Etching condition: source power: 2500W, bias power 150W, gas pressure: 5 mTorr, and gas flow rate: 40sccm.)                                  90
Figure 4-9      Etch rates of PtOx and PZT and their etching selectivity as a function of O2 content in the Ar/(50％)CF4/O2 plasma. (Etching condition: source power: 2500W, bias power 150W, gas pressure: 5 mTorr, and gas flow rate: 40sccm.)                                      91
Figure 4-10      SEM micrographs of PtOx/PZT capacitor stacks. The PZT films were etched in (a) Ar/ (10％)O2/(30％)Cl2 plasma and in (b) Ar / (50％)CF4/ (30％)O2 plasma. The slope of the sidewall capacitor is 72°.        92
Figure 4-11      Comparison of P-E hysteresis loops of 100×100μm2 PtOx /PZT capacitors etched with the O2 gas added to Ar/(50％) CF4 plasma.  93
Figure 4-12      (a) Comparison of fatigue characteristics of 100×100μm square PtOx /PZT capacitor stacks etched with the O2 gas added to Ar/(50％) CF4 plasma. Inset showed the fatigue characteristics of (b) the polarization switching current density and (c) P-E hysteresis loops for PtOx /PZT capacitors etched in Ar/(30％) CF4 /(50％) CF4 plasma. The applied voltage was 5V and operated at a frequency of 1 MHz.
94
Figure 4-13      X-ray photoelectron spectra for the comparison with O2 gas addition (a) Pb4f electrons (b) Zr3d electrons and (c) Ti2p electrons from etched PZT films.                                                95
Figure 4-14      Atomic concentration of etched PZT capacitors with the various O2 concentrations in Ar/(50％) CF4 plasma                        97
Figure 5-1      RBS spectra for scattering 2Mev He2+ ions from different stoichiometric PtOx films on Ti/Si substrate. The films with Ar/O2= 90/10 and 70/30 gas mixture ratio corresponded with stoichiometric Pt/O=1/0.4 and Pt/O=1/1, respectively.                        115
Figure 5-2      RBS spectra for scattering 2Mev He2+ ions of stoichiometric Pb(Zr0.4 Ti0.6)O3 films on Si substrate.                                115
Figure 5-3      Comparison of P-V hysteresis loops of Pt/PZT/Pt capacitors with different forming gas annealing time at 200℃.                  116
Figure 5-4      Comparison of P-V hysteresis loops of (a) PtO0.4/PZT /Pt capacitors and (b) PtO/PZT /Pt capacitors with different forming gas annealing time at 200℃.                                             117
Figure 5-5      Remanent polarization of PtO/PZT/Pt capacitor cell size dependence after forming gas annealing at 200℃. 30min. The inset show (b) P-V hysteresis loops measured by AFM for 0.25μm2 capacitors before and after annealing. (c) SEM micrograph of PZT capacitor stack.    118
Figure 5-6      SIMS depth profiles of hydrogen-treated (a) PtO/PZT/Sub and(b) Pt/PZT/Sub specimens. Hydrogen annealing was performed at 200℃ for 15min.                                                119
Figure 5-7      ERD spectra for scattering 2.7Mev He2+ ions from blanket Pt/PZT/Pt configurations with different annealing time at 200℃ (a) 15min (b) 30min (c) 45min.                                           120
Figure 5-8      Energy diagrams for the PtOx/PZT capacitor; (a) before H2 treatment and (b) after H2 treatment. When the injected hydrogen trapped at Pt/PZT interface, the defect act as donors and provides electrons due to the high work function of Pt, causing the development of a negative built-in voltage and bending of band in PZT.                   121
Figure 5-9      ERD spectra for scattering 2.7Mev He2+ ions from different blanket top electrode(a) PtO/PZT (b)PtO0.4/PZT (c)Pt/PZT configurations annealing at 200℃ for 30min.                               122
Figure 5-10      X-ray photoelectron spectra of (a) Pt4f and (b) O1s electrons obtained from the PtO/PZT/Pt capacitor specimen before and after H2 annealing at 200℃ for 15min; Oads denotes the adsorbed oxygen, and Os the oxygen incorporated in the PtOx film.                   123
Figure 5-11      The work function differences of PtOx films with varied stoichiometric compositions before and after forming gas annealing at 200℃ 15min. Inset exhibited work function differences of PtO films measured by photoelectron spectrometer.                                 124
Figure 5-12      J-V characteristics of hydrogen-treated PZT capacitors with different top electrode at 298K. The forming gas annealing was performed at 200℃ for 15min.                                          125
Figure 5-13      Temperature dependence of J-V characteristics from PZT capacitors with different top electrode. (a) PtO/PZT/Pt capacitor before forming gas annealing. (b) PtO/PZT/Pt capacitors after forming gas annealing at 200℃ for 15min. (c) Pt/PZT/Pt capacitor before forming gas annealing. (d) Pt/PZT/Pt capacitors after forming gas annealing at 200℃ for 15min.                                             126
Figure 5-14      Schottky emission Plots of ln(J/T2) vs (V1/2) at an intermediate voltage from 1V to 7.84 V with different specimens. (a) PtO/PZT/Pt capacitor before annealing. (b) PtO/PZT/Pt capacitors after annealing at 200℃ for 15min. (c) Pt/PZT/Pt capacitor before forming gas annealing. (d) Pt/PZT/Pt capacitors after forming gas annealing at 200℃ for 15min.
128
Figure 5-15      Plots of ln(J/T2)V=0 Vs. (1/T) from specimens (a) PtO/PZT/Pt capacitors and (b) Pt/PZT/Pt capacitors before and after annealing. The Schottky barrier height can be derived from the Arrhenius plot of ln(J/T2)V=0 Vs. (1/T).                                        130
Figure 5-16      Diagram showing sign of screen charge on the electrode when polarization is in the same direction as the applied electric field and vice-versa.                                                131
Figure 5-17      Energy band diagram of a metal-n- type semiconductor contact with an interfacial layer. ψm: work function of metal, ψBn : barrier height of m-s surface barrier, ψ0: energy level at surface defined in (5-5), ψn: energy difference between conduction band and Fermi level in bulk semiconductor, △ψn: image force barrier lowering, Eg: energy gap of semiconductor, εi: dielectric constant of interfacial layer, εs: dielectric constant of semiconductor, χs: electron affinity, δ: thickness of interfacial layer, Qm: surface charge density on mental, Qss surface state charge density on semiconductor, Qsc :space charge density in semiconductor.                                            131
Figure 5-18      Calculation Schottky barrier height variation against interfacial doping concentration for hydrogen treated (a) PtO electrode and (b) Pt electrode.                                               132
Figure 6-1      Schematic diagram of the VT Beam Deflection AFM 25.          143
Figure 6-2      XRD diffraction patterns of PtOx/PZT/PtOx/Pt thin films structure deposited and followed by the annealing process for crystallization.
144
Figure 6-3      Dependence of the critical dimension of NEB resist dot size with variation of exposure electron-beam dosages.                  145
Figure 6-4      Etch rate of PtOx and NEB and their etching selectivity as a function of O2 content in the Ar/(20％)Cl2/O2 plasma.                   146
Figure 6-5      Etch rates of PZT and NEB and their etching selectivity as a function of O2 content in the Ar/(50％)CF4/O2 plasma.                  146
Figure 6-6      SEM micrographs showing (a) array (b) single cell capacitor of 500nm lateral size.                                               147
Figure 6-7      SEM micrographs showing (a) array (b) single cell capacitor of 300nm lateral size                                               148
Figure 6-8      SEM micrographs showing (a) array (b) single cell capacitor of 200nm lateral size                                               149
Figure 6-9      SEM micrographs showing (a) array (b) single cell capacitor of 180nm lateral size.                                               150
Figure 6-10      SEM micrographs showing (a) array (b) single cell capacitor of 150nm lateral size.                                               151
Figure 6-11      SEM micrographs showing (a) array (b) single cell capacitor of 90nm lateral size.                                               152
Figure 6-12      Cross-section view SEM micrographs of PtOx /PZT capacitors with (a) 150nm (b) 90nm feature size.                                153
Figure 6-13      (a) AFM surface morphology image and (b) SCM image after domain patterning at (dC/dV) =0 was obtained from 2μm square PZT capacitor.                                                154
Figure 6-14      Comparison of P-V hystersis loops obtained from PtOx /PZT capacitor stacks with 0.09× 0.09μm2 feature size. (a) Before compensated with open measurement and (b) after compensation. Clear hystersis loops were exhibited.                                            155
Figure 6-15      Comparison of P-V hystersis loops with different capacitors feature size.                                                     156
Figure 6-16      P-V hysteresis loops of 0.2 ×0.2μm2  capacitors at various temperature.                                             157

                                

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