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研究生：	翁崇銘 Weng, Chung-Ming
論文名稱：	高功率無鉛壓電元件之開發：無鉛鈮酸鈉鉀基壓電陶瓷製備、元件設計及整合 Development of Lead-free Piezoelectric Devices with High Power: Preparations of Lead-free (NaxK1-x)NbO3-based Piezoelectric Ceramics、Component Design and Devices Integration
指導教授：	朱聖緣 Chu, Sheng-Yuan
學位類別：	博士 Doctor
系所名稱：	電機資訊學院 - 電機工程學系 Department of Electrical Engineering
論文出版年：	2018
畢業學年度：	107
語文別：	英文
論文頁數：	147
中文關鍵詞：	無鉛壓電陶瓷、高機械品質因子、壓電元件
外文關鍵詞：	Lead-free piezoelectric ceramics, High mechanical quality factor, Piezoelectric Device
相關次數：	點閱：60 下載：0
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本論文採用固態反應法製備無鉛鈮酸鈉鉀基（NKN-based）壓電陶瓷，藉由適當的摻雜少量氟化銅（CF）和鈮酸鋰（LN）燒結促進劑，探討其對陶瓷的微觀結構ヽ氧空位ヽ電性能和穩定性之影響。用CF和LN燒結促進劑所合成之壓電陶瓷，比起純鉛鈮酸鈉鉀陶瓷具有更高的密度，並在不同的濕度環境下，還能保持相當穩定的電特性。此外，在本論文中已證明所添加之燒結促進劑（CF和LN）能夠有效的降低最佳燒結溫度。NKNCF陶瓷能在燒結溫度1000度時，表現出優越的“硬”壓電特性：kp = 35%，kt = 45%，k33 = 55%，d33 = 88 pC/N，Qm = 2800，以及 tanδ = 0.1%。相比之下， NKLN陶瓷在燒結溫度950度時，能獲得良好的“軟”壓電特性：kp = 50%，kt = 53%，k33 = 68%，d33 = 150 pC/N，Qm = 168，以及 tanδ = 4%。
其次，本論文使用新型燒結促進劑水合氟化铜(CH)製備無鉛鉛鈮酸鈉鉀基陶瓷，研究其在不同後退火處理溫度與氣氛下，對陶瓷材料的氧空位ヽ微觀結構和電性能之影響。 NKNCH陶瓷在氬氣下後退火處理800度時，可使其相對密度增加到97％。所得樣品呈現出以下優異的壓電性能：kp = 34.1%，kt = 45.3%，Qm = 3170，Rz = 8.6Ω，以及 tanδ = 0.1%。實驗結果清楚的表明，壓電陶瓷在適當的溫度與氬氣下後退火處理，將可以有效的再次產生氧空位，這對陶瓷材料的域結構之穩定性具有顯著的影響。據我們所知，這是第一篇報導無鉛壓電陶瓷添加CF和CH燒結促進劑的論文。
最後，本論文將所開發出的壓電陶瓷，分別用於製造3MHz超音波治療傳感器ヽ表面聲波元件和線性超音波馬達，並探討其元件之性能。實驗結果清楚地表明，3MHz超音波治療傳感器在元件聲功率的探討中，其元件之RzヽQm和tanδ的值，比其機電耦合係數（k）更為重要的作用。 “硬”性NKNCF陶瓷相較於“軟”性NKLN陶瓷，其較容易產生更大的聲功率，這將促使它更適用於超音波治療傳感器之應用。表面聲波元件採用所提出之NKLN陶瓷製造，其呈現出良好的元件特性：波速為3210 m/s，機電轉換效率(k2)為6.7%，TCF約為−282 ppm/℃。即使在濕度變化很大的情況下，其元件也表現出良好的穩定性。壓電馬達採用所提出之NKNCH陶瓷製造，其馬達表現出高的水平速度為4.5 mm/s與垂直速度為3.02 mm/s。此外，當壓電馬達驅動時，其可表現出相當低的元件溫升，在驅動三分鐘時即可達到穩定。這結果表明，在未來高功率壓電元件製造中，無鉛NKNCH陶瓷將有機會可以替代PZT壓電陶瓷。

In this thesis, CuF2 (CF) and LiNbO3 (LN) modified lead-free (Na, K)NbO3 (NKN)-based ceramics (NKNCF and NKLN) were synthesized using solid-state reaction methods. The influence of doping materials on the microstructure, oxygen vacancies, electrical properties, and stability of the synthesized ceramics was then investigated. The ceramics synthesized with CF and LN dopants were of higher density than pure NKN ceramics and far more stable under different temperature and humidity. Moreover, the addition of sintering aids (CF and LN) had been proven particularly effective in reducing the optimal sintering temperature. NKNCF ceramics sintered at 1000℃ exhibited excellent “hard” piezoelectric properties (kp = 35%, kt = 45%, k33 = 55%, d33 = 88 pC/N, Qm = 2800, and tanδ = 0.1%). In contrast, NKLN ceramics sintered at 950℃ exhibited excellent “soft” piezoelectric properties (kp = 50%, kt = 53%, k33 = 68%, d33 = 150 pC/N, Qm = 168, and tanδ = 4%). The proposed ceramic materials are ideally suited to electromechanical devices for use in a wide variety of environments.
Secondly, Lead-free NKN ceramics were prepared using a novel sintering aid (CuF2．xH2O (x≈2)) to investigate the effects of post-annealing temperature and atmosphere on oxygen vacancies, microstructure, and electrical properties. Post-annealing NKN + 1.5mol% CuF2．xH2O (CH) ceramics at 800℃ under argon was shown to increase the bulk relative density to 97% through the formation of a homogeneous microstructure with liquid phase. The resulting samples presented the following excellent piezoelectric properties: kp：34.1%; kt：45.3%; Qm：3170; Rz：8.6Ω; and tanδ：0.1%. Our results clearly demonstrate that annealing under argon can produce oxygen vacancies in ceramics, which has a significant influence on the stability of domain structures of the samples. To the best of our knowledge, this is the first paper reporting on the addition of CF and CH dopants to lead-free piezoelectric ceramics.
Finally, the proposed ceramics were then used in the fabrication of 3-MHz ultrasonic therapeutic transducers, surface acoustic wave (SAW) devices, and rotary-linear ultrasonic motors, respectively. Moreover, the performances of piezoelectric devices for NKN-based ceramics were also investigated. Our results clearly demonstrate that the Rz, Qm and tanδ play a more important role in the generation of acoustic power of ultrasonic therapeutic transducers than the electromechanical coupling coefficient (k). The NKNCF ceramics were found to easily generate a greater acoustic power, which makes them suitable for applications in therapeutic transducers. SAW devices fabricated using the proposed NKLN ceramics presented high phase velocity of 3210 m/s, k2 of 6.7%, and TCF of approximately −282 ppm/℃. The resulting device demonstrated excellent stability, even under the effects of large variations in humidity. This material could be applied in electromechanical transducers as well as a wide range of SAW temperature sensors, thanks to the sensitivity provided by high k2 values and high phase velocity. Piezoelectric motors fabricated using the proposed NKNCH ceramics achieved a high level velocity of 4.5 mm/s, vertical velocity of 3.02 mm/s, and output power of 2.93 mW. The resulting device exhibited a moderate increase in operating temperature, reaching a stable plateau when the motor was driven for three min. These results demonstrate the potential of using lead-free NKNCH ceramics as an alternative to PZT-based ceramics in the further development of high-power piezoelectric devices.

Abstract................................................I
中文摘要...............................................III
致謝....................................................V
List of Author’s Journal Paper Publications............VI
Table of Contents....................................VIII
List of Figures.......................................XII
List of Tables........................................XIX
Chapter 1: Introduction.................................1
1 Piezoelectric materials.............................1
2 Application on ultrasonic therapeutic transducers...4
3 Application on surface acoustic wave devices........5
4 Application on rotary-linear ultrasonic motors......5
5 Aims of the thesis..................................6
Chapter 2: Theories and Literature Reviews..............9
1 Piezoelectric effects...............................9
2 Piezoelectric Constitutive Equations...............10
3 Structure of piezoceramics.........................12
3.1 Perovskite-type structure........................12
3.2 Domain structure.................................12
3.3 Piezoelectric resonator..........................13
4 Sodium potassium niobate...........................14
5 Mechanism of low-temperature sintering.............15
6 Ferroelectrics.....................................16
7 Mechanism of hardening effect and phenomenon.......16
8 Arrhenius law and relaxation time of polarization..17
9 Finite Element Method..............................18
10 Ultrasonic therapeutic transducers................19
10.1 Mason model and input electrical impedance of transducers............................................19
10.2 Acoustic matching theorem.......................23
11 Bulk and surface acoustic wave....................24
11.1 Piezoelectric interactions......................24
11.2 Rayleigh wave considerations....................25
11.3 Structure of surface acoustic wave device.......26
11.4 Cross-field model...............................27
12 Rotary-linear ultrasonic motors...................27
Chapter 3: Experimental Procedures and Measurements....36
1 Preparation of piezoelectric ceramics..............36
2 Measurements of microstructure properties..........38
2.1 Bulk density analysis............................38
2.2 X-ray diffraction analysis.......................38
2.3 X-ray photoelectron spectroscopy analysis........38
2.4 SEM and EDS analysis.............................38
3 Measurements of electrical properties..............39
3.1 Dielectric constant..............................39
3.2 The Curie temperature (TC).......................39
3.3 Electrochemical coupling factor (k)..............39
3.4 Mechanical quality factor (Qm)...................40
3.5 Piezoelectric coefficient (d33)..................40
3.6 Frequency constant...............................41
3.7 Ferroelectric hysteresis loops...................41
3.8 Temperature coefficient of frequency.............41
3.9 Energy activation (Ea)...........................42
4 The fabrication of therapeutic transducers.........42
5 The fabrication of SAW properties..................42
5.1 Phase velocity...................................43
5.2 Electromechanical coupling coefficient...........43
6 The fabrication of rotary-linear ultrasonic motors.43
Chapter 4: Characterizations of (NaxK1-x)NbO3 Based Lead-Free Ceramics..........................................52
1 Effects of CuF2 dopant.............................52
1.1 Microstructure analysis and bulk density.........52
1.2 Analysis of electrical properties................55
2 Effects of LiNbO3 dopant...........................62
2.1 Microstructure analysis and bulk density.........63
2.2 Analysis of electrical properties................64
3 The stability of NKNCF and NKLN ceramics...........66
4 Effects of post-annealing on CuF2・xH2O (x ≈ 2) dopant.................................................69
4.1 Microstructure analysis and bulk density.........69
4.2 Analysis of electrical properties................71
Chapter 5 The Application of Lead-Free Piezoelectric Ceramics...............................................99
1 Ultrasonic therapeutic transducers: Resistance to temperature and humidity...............................99
1.1 Introduction.....................................99
1.2 Results and discussion...........................99
2 Surface acoustic wave devices.....................102
2.1 Introduction....................................102
2.2 Results and discussion..........................103
3 Rotary-linear ultrasonic motors...................104
3.1 Introduction....................................104
3.2 Results and discussion..........................105
Chapter 6: Summary and Recommendations for Future Work..................................................123
1 Summary...........................................123
1.1 Piezoelectric ceramics..........................123
1.2 Piezoelectric devices...........................125
2 Suggestions for future work.......................126
References............................................127

                                    

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