磁控濺鍍BZT/(Ta2O5)1-x(TiO2)x薄膜為MFIS微波變容器之高頻與微波頻段特性研究

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研究生：	王參群 Tsan-Chun Wang
論文名稱：	磁控濺鍍BZT/(Ta2O5)1-x(TiO2)x薄膜為MFIS微波變容器之高頻與微波頻段特性研究 High Frequency and Microwave Characteristics of BZT/(Ta2O5)1-x(TiO2)x Thin Films deposited by RF Magnetron sputtering for MFIS varactors
指導教授：	吳泰伯 Tai-Bor Wu
口試委員:
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2006
畢業學年度：	94
語文別：	中文
論文頁數：	151
中文關鍵詞：	鐵電、鋯鈦酸鋇、緩衝層、氧化鈦、氧化鉭、變容器、微波
相關次數：	點閱：3 下載：0
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本實驗以磁控濺鍍法鍍製BZT/ (Ta2O5)1-x(TiO2)x薄膜於高阻值Si基板(n-type,電阻率~5000Ω-cm)上，製作具有high-k介電緩衝層之MFIS(metal-ferroelectric-insulator-semiconductor)變容器，觀測其在高頻(1MHz)與微波頻段(50MHz to 25 GHz)下的特性，並探討此特性與製程條件、熱處理過程之關係。高介電常數緩衝層的置入一般被認為可以提升薄膜的有效介電常數並降低微波能量在矽基板的損耗，使得此結構可應用於矽基整合鐵電微波元件上。矽基整合製程為利用製程穩定性高、控制容易、技術成熟的半導體製程將薄膜型被動元件整合在單一晶片上，可滿足高頻通訊被動元件嚴格之規格要求。
實驗結果發現BZT/(Ta2O5)1-x(TiO2)x /HRS結構之MFIS變容器其大部分的調變性在高頻部分是來自於1.Si基板表面因為偏壓施加所顯現的半導體特性和2.因高溫鍍製BZT所造成的緩衝層金屬離子氧化態改變以及對應產生的離子空缺和載子效應。這些在製程中(鍍膜條件、退火溫度、氛圍)不易避免的現象將會使得單一Metal-Oxide-Semiconductor(MOS)的平帶電壓產生偏移，使得兩個back-to-back串接而成C-V圖顯現出製程相關的結果，並反應在不同的極值電容值及迥異的loss-V圖，同時也影響到微波頻段的特性。而在微波頻段中比較低頻的區間其特性是基板性質控制，隨著頻率增加至25GHz，逐漸的轉為順電相調變層與緩衝層控制。顯然的在微波頻段較高頻率的區間，調變性比1MHz時所量測到的小許多，但仍有28.70%( BZT500nm 600℃ /(Ta2O5)0.929(TiO2)0.071 50nm 200℃ /HRS、頻率25GHz、DC bias 32V)之調變能力，於是我們認為未來如果能將製程條件再做改善達到最佳化，將可以成功的將此高調變性薄膜導入矽□半導體製程產業中，真正達到降低生產成本、推廣鐵電材料在微波頻段應用於varactor, filter, phase shifter或其他元件的目的。

                          目  錄
摘要...................................................... I
致謝.................................................... III
目錄..................................................... IV
表目錄................................................... VI
圖目錄................................................... VI
第一章 緒論................................................1
   1.1 前言................................................1
   1.2 動機與目標..........................................2
第二章 文獻回顧............................................6
   2.1 矽基板整合鐵電材料之微波元件........................6
     2.1.1 鐵電材料應用於微波元件的優勢................... 7
     2.1.2 整合製程...................................... 10
     2.1.3 矽基板之優點與特性.............................11
     2.1.4 Si基板整合鐵電變容器...........................11
     2.1.5 高阻值矽基板...................................13
   2.2鐵電材料的研究與發展............................... 14
     2.2.1鐵電材料的結構與特性........................... 14
     2.2.2 鈦酸鋇系鐵電材料.............................. 16
     2.2.2-1鈣鈦礦結構................................... 16
     2.2.3-2鈦酸鋇........................................17
     2.2.2-3鋯鈦酸鋇(Ba(Zr,Ti)O3，BZT) ...................18
     2.3(Ta2O5)1-x(TiO2)x的研究及發展.....................18
     2.3.1單成分介電材料發展緣由..........................18
     2.3.2 (Ta2O5)1-x(TiO2)x薄膜..........................20
   2.4極化機制............................................21
     2.4.1 極化現象...................................... 22
     2.4.2 介電常數與介電損失............................ 23
   2.5 鐵電薄膜/緩衝層在Si基板共平面結構上的電性機制......24
   2.6微帶結構電容模型—CAD model.........................26
第三章 實驗方法與步驟.....................................45
   3.1緩衝層薄膜之製備................................... 45
     3.1.1(Ta2O5)1-x(TiO2)x緩衝層靶材製備.................45
     3.1.2(Ta2O5)1-x(TiO2)x薄膜...........................46
   3.2 BZT薄膜之製備......................................47
     3.2.1 BZT靶材....................................... 47
     3.2.2 BZT薄膜........................................48
   3.3薄膜熱處理......................................... 48
     3.3.1 (Ta2O5)1-x(TiO2)x /HRS結構退火製程.............48
     3.3.2 BZT/(Ta2O5)1-x(TiO2)x /HRS結構退火製程.........48
   3.4上電極之製作....................................... 49
     3.4.1 Wet etching法..................................49
   3.5薄膜分析量測........................................50
     3.5.1 薄膜結構分析...................................50
     3.5.2 薄膜成分分析.................................. 50
     3.5.3厚度量測及微觀結構—SEM分析.....................51
     3.5.4電性分析..................... ..................51
     3.5.6穿透式電子顯微鏡及Energy Dispersive Spectrometer  (EDS) ................................................... 53
     3.5.7 Energy Spectroscope for Chemical Analysis (ESCA)....................................................53
第四章 結果與討論.........................................64
   4.1 (Ta2O5)1-x(TiO2)x薄膜特性..........................64
     4.1.1成分對薄膜電性之影響............................64
     4.1.2退火對薄膜電性之影響............................65
   4.2 BZT薄膜特性........................................65
     4.2.1 BZT薄膜成分鑑定................................65
     4.2.2 鍍膜溫度對高頻(1Mhz)電性之影響.................66
   4.3 各種缺陷電荷對於BZT/(Ta2O5)1-x(TiO2)x/HRS結構之電性影響........................................................67
     4.3.1 Oxide trapped charge之影響.....................68
     4.3.2 Mobile  ion  charge 之影響.....................69
     4.3.3 Fixed oxide charge  之影響.....................69
     4.3.4 緩衝層氧化物還原之貢獻.........................70
   4.4 BZT/(Ta2O5)1-x(TiO2)x/HRS結構之高頻、微波特性討論..72
     4.4.1 BZT鍍膜溫度、緩衝層介電常數對BZT/(Ta2O5)1-x(TiO2)x薄膜電性之影響.......................................... 72
     4.4.2 緩衝層成分、膜厚對薄膜電性之影響.............. 77
     4.4.3 退火氛圍對薄膜電性之影響...................... 80
   4.5 正反調變性機制模型.................................83
     4.5.1 Lightly-Depleted...............................85
     4.5.1.1施加小偏壓下..................................85
     4.5.1.2施加大偏壓下..................................85
     4.5.2 Heavily-Depleted...............................86
     4.5.2.1施加小偏壓下..................................86
     4.5.2.2施加大偏壓下.. ...............................87
   4.6 以HFSS模擬BZT/(Ta2O5)1-x(TiO2)x/HRS結構............87
     4.6.1 HFSS模擬之結構.................................87
     4.6.2 HFSS模擬結果...................................88
第五章 結論..............................................145
第六章 參考文獻..........................................147


表目錄
表1.1 行動通訊系統之發展...................................5
表1.2 鐵電膜在微波調諧元件應用之優勢比較...................5
表2.1 各種變容器的比較....................................43
表2.2 三十二種晶體點群對稱............................... 43
表2.3 (Ta2O5)1-x(TiO2)x塊材1MHz下的介電常數和散逸因子.....44
表3.1 (Ta2O5)1-x(TiO2)x薄膜之濺鍍條件.....................62
表3.2 BZT薄膜之濺鍍條件...................................62
表3.3 Ag上電極之濺鍍條件.......................... .......63
表4.1 (Ta2O5)1-x(TiO2)x以及BZT之靶材、薄膜成分...........141
表4.2 (Ta2O5)1-x(TiO2)x以及BZT之靶材之鍍率...............141
表4.3 BZT(500nm)/buffer(50nm 200℃鍍膜)/HRS在不同BZT鍍膜溫
度下的高頻、微波頻段特性列表......... ...................142
表4.4 BZT/buffer/HRS在不同緩衝層膜厚下的高頻、微波頻段特性
列表.....................................................143
表4.5 BZT/buffer/HRS在不同熱處理條件下的微波頻段(2GHz)特性列表.......................................................144

圖目錄
圖1.1 各類訊號傳輸內容比重隨時間演進................... ...4
圖2.1 鐵電材料電容-電壓曲線圖：(a).鐵電相；(b).順電相.....29
圖2.2 Si(a)頻率對阻值的作圖﹔(b)loss tanδ對頻率作圖......29
圖2.3 四種基本共振線路................................. ..30
圖2.4 主動元件與被動R、L、C元件之積體化電路...............30
圖2.5 相位陣列天線示意圖..................................31
圖2.6 在Si基板上共平面結構之鐵電變容器(MIS structure) ... 31
圖2.7 平行電板結構(MIM structure)之變容器.................32
圖2.8 平行電容與共平面電容比較........................... 32
圖2.9 共平面結構的等效電路............................... 33
圖2.10 MFOS與MOS的比較..................................  33
圖2.11 鐵電MIM結構與Si變容器之Q factor的比較..............34
圖2.12 鐵電MFOS結構與有無緩衝層之損耗示意圖......... ...  34
圖2.13 典型鐵電材料之電滯曲線圖...........................35
圖2.14 典型ABO3鈣鈦礦之晶體構造示意圖.....................35
圖2.15 鈦酸鋇相轉變之結晶構造與溫度關係圖.................36
圖2.16 等價取代離子對鈦酸鋇晶格轉換溫度之影響圖......... .36
圖2.17 DPT行為1及正常鐵電行為2：(a)自發極化對溫度，(b)介電常數對溫度，(c)介電常數對頻率關係圖.........................37
圖2.18 (Ta2O5)1-x(TiO2)x介電常數對TiO2莫爾添加量之關係....37
圖2.19 材料的四種極化機構簡圖.............................38
圖2.20 材料之介電常數隨頻率的變化圖.......................39
圖2.21鐵電薄膜在Si基板共平面結構之等效電路圖；(a)小dc偏壓之下；(b)大dc偏壓之下；(c)微波頻段等效電路..................39
圖2.22 MFOS薄膜結構電極2施加由正到負的電壓其電容電壓圖....40
圖2.23 (a)電極1下的C-V圖  (b)C1與C2兩者串聯合併...........40
圖2.24 低頻與高頻之C-V變化................................41
圖2.25 (a)三層基板之金屬微帶結構、(b)等效電路以及(c)電磁場分布.............. .........................................41
圖2.26多層基板之金屬微帶結構..............................42
圖3.1 實驗流程............................................54
圖3.2 退火熱處理實驗流程...................... ...........54
圖3.3 (Ta2O5)1-x(TiO2)x靶材配製之流程圖...................55
圖3-4(a) (Ta2O5)1-x(TiO2)x粉末煆燒溫度曲線................56
圖3-4(b) (Ta2O5)1-x(TiO2)x靶材燒結溫度曲線................56
圖3.5 BaZrO3粉末煆燒後之XRD................... ...........57
圖3.6 Ba2TiO4粉末煆燒後之XRD..............................57
圖3.7 BZT粉末(Ba未過量)煆燒後之XRD........................58
圖3.8 BZT粉末(Ba過量)煆燒後之XRD.................. .......58
圖3.9  Ba2TiO4、BaZrO3、BZT(Ba未過量)粉末配製之流程圖.....59
圖3.10 Ba-rich BZT靶材配製流程圖................... ......59
圖3.11黃光微影法製作指叉和方塊上電極的圖樣................60
圖3.12上電極的圖樣........................................60
圖3.13指叉與方塊共平面電極結構側視圖......................61
圖3.14 信號流動圖形(one-port) ............................61
圖4.1 Ag/(Ta2O5) /Pt/Ti/Si結構之高頻電性..................89
圖4.2 Ag/(Ta2O5)0.929(TiO2)0.071  /Pt/Ti/Si結構之高頻電性.89
圖4.3 Ag/(Ta2O5)0.8(TiO2) 0.2/Pt/Ti/Si結構之高頻電性......90
圖4.4 Ag/(Ta2O5)1-x(TiO2)x/Ti/Pt/Si結構，以電性對target成分之作圖................... ........................ .......90
圖4.5 (a)(b)(c)各別代表成分為x=0、x=0.08、x=0.16的(Ta2O5)1-x(TiO2)x靶材在表3.1條件下鍍膜在Pt/Ti/SiO2/Si基板上一個小時之SEM截面影像...............................................92
圖4.6 (a)(b)為x=0、x=0.08的靶材在表3.1條件下鍍膜於白金鈦基板上，經熱處理後(氧氣)，介電常數對熱處理溫度關係圖..........93
圖4.7 (a)(b) x=0、x=0.08的靶材在表3.1的條件下鍍膜在Pt/Ti/SiO2/Si上，經熱處理後(氧氣)，其結晶繞射結果........................................................94
圖4.8 C-V and Loss-V characteristics of BZT film deposited at 500℃(1MHz) ..........................................95
圖4.9 C-V Loss-V characteristics of BZT film deposited at 600℃(1MHz) ................... ..........................95
圖4.10 C-V Loss-V characteristics of BZT film deposited at 700℃(1MHz) ............................. ................96
圖4.11(a) 不同鍍膜溫度的BZT薄膜之Xray繞射結果(去除Pt繞射峰)(b)調變性、FOM與鍍膜溫度之關係............ ...............97
圖4.12 偏壓施加下，介面電荷情況...........................97
圖4.13 oxide中各種charge之分佈............................98
圖4.14 電極2施加負偏壓，oxide中trap電子造成C2-V圖偏移.....98
圖4.15 gate injection時，電極2施加電壓造成的C-V圖.........99
圖4.16 substrate injection時，電極2施加電壓造成的C-V遲滯..99
圖4.17 Mobile ion charge在電極2施加負電壓時的電荷分布....100
圖4.18電極2施加電壓，mobile ion charge造成的C-V現象......100
圖4.19 Fixed Oxide charge................................101
圖4.20 電極2施加偏壓，正fixed oxide charge影響C1、C2串接結果.............. ........................................101
圖4.21 Ta-Si-O 以及 Ti-Si-O三元相圖(temperature=700-1000℃) ..................... ...........................102
圖4.22 Ta2O5 (10nm 200℃)/HRS仿照BZT鍍膜條件熱處理後，其ESCA縱深分析結果............. ...............................103
圖4.23 BZT鍍膜溫度為500℃之BZT/Ta2O5/HRS結構C-V高頻特性圖.................. ....................................104
圖4.24 BZT鍍膜溫度為500℃之BZT/Ta2O5/HRS結構LOSS-V高頻特性圖................ ...................... ...............104
圖4.25 BZT鍍膜溫度為600℃之BZT/Ta2O5/HRS結構C-V高頻特性圖................................. .....................105
圖4.26 BZT鍍膜溫度為600℃之BZT/Ta2O5/HRS結構LOSS-V高頻特性圖.......................... ............................105
圖4.27 BZT鍍膜溫度為700℃之BZT/Ta2O5/HRS結構C-V高頻特性圖.......................... ............................106
圖4.28 BZT鍍膜溫度為700℃之BZT/Ta2O5/HRS結構LOSS-V高頻特性圖.......................  ..............................106
圖4.29 BZT鍍膜溫度為500℃之BZT/(Ta2O5)0.929(TiO2)0.071  /HRS結構C-V高頻特性圖........................................107
圖4.30 BZT鍍膜溫度為500℃之BZT/(Ta2O5)0.929(TiO2)0.071  /HRS結構LOSS-V高頻特性圖.....................................107
圖4.31 BZT鍍膜溫度為600℃之BZT/(Ta2O5)0.929(TiO2)0.071  /HRS結構C-V高頻特性圖.......... .............................108
圖4.32 BZT鍍膜溫度為600℃之BZT/(Ta2O5)0.929(TiO2)0.071  /HRS結構LOSS-V高頻特性圖.....................................108
圖4.33 BZT鍍膜溫度為700℃之BZT/(Ta2O5)0.929(TiO2)0.071  /HRS結構C-V高頻特性圖........................................109
圖4.34 BZT鍍膜溫度為700℃之BZT/(Ta2O5)0.929(TiO2)0.071  /HRS結構LOSS-V高頻特性圖.....................................109
圖4.35 XRD result of BZT/(Ta2O5)0.929(TiO2)0.071  /HRS structure；BZT thin films were deposited at 500℃、600℃、700℃....................................................110
圖4.36 XRD result of BZT/(Ta2O5) /HRS structure；BZT thin films were deposited at 500℃、600℃、700℃...... .............................................110
圖4.37 back-to-back simulation results of C-V curve，(a)(b)(c) correspond to different C-V curves with increasing positive oxide fixed charge(decreasing negative oxide fixed charge) .................................................111
圖4.38 C-f and Loss-f performance of BZT(500nm 500℃)/Ta2O5(50nm 200℃)/HRS structure at Microwave frequency........112
圖4.39 C-f and Loss-f performance of BZT(500nm 600℃)/Ta2O5(50nm 200℃)/HRS structure at Microwave frequency........113
圖4.40 C-f and Loss-f performance of BZT(500nm 700℃)/Ta2O5(50nm 200℃)/HRS structure at Microwave frequency........114
圖4.41 C-f and Loss-f performance of BZT(500℃ 500nm)/(Ta2O5)0.929(TiO2)0.071 (50nm 200℃)/HRS structure at Microwave frequency... ..................................115
圖4.42 C-f and Loss-f performance of BZT(600℃ 500nm)/(Ta2O5)0.929(TiO2)0.071 (50nm 200℃)/HRS structure at Microwave frequency................................. ....116
圖4.43 C-f and Loss-f performance of BZT(700℃ 500nm)/(Ta2O5)0.929(TiO2)0.071 (50nm 200℃)/HRS structure at Microwave frequency......................................117
圖4.44 BZT(600℃500nm)/Ta2O5(50nm)/HRS結構LOSS-V高頻特性圖.......................................................118
圖4.45 BZT(600℃500nm)/Ta2O5(100nm)/HRS結構LOSS-V高頻特性圖.......................................................118
圖4.46 BZT(600℃500nm)/Ta2O5(200nm)/HRS結構LOSS-V高頻特性圖.......................................................119
圖4.47 BZT(600℃ 500nm)/ (Ta2O5)0.929(TiO2)0.071 (50nm)/HRS結構LOSS-V高頻特性圖...................... ..............119
圖4.48 BZT(600℃500nm)/ (Ta2O5)0.929(TiO2)0.071 (100nm)/HRS結構LOSS-V高頻特性圖.....................................120
圖4.49 BZT(600℃ 500nm)/ (Ta2O5)0.929(TiO2)0.071 (200nm)/HRS結構LOSS-V高頻特性圖.....................................120
圖4.50 XRD results of BZT(600℃ 500nm)/Ta2O5(50nm、100nm、200nm)/HRS...............................................121
圖4.51 XRD results of BZT(600℃ 500nm)/ (Ta2O5)0.929(TiO2)0.071 (50nm、100nm、200nm)/HRS...........................121
圖4.52 C-f and Loss-f performance of BZT(500nm 600℃)/Ta2O5(50nm)/HRS structure at Microwave frequency..............122
圖4.53 C-f and Loss-f performance of BZT(500nm 600℃)/Ta2O5(100nm)/HRS structure at Microwave frequency.............123
圖4.54 C-f and Loss-f performance of BZT(500nm 600℃)/Ta2O5(200nm)/HRS structure at Microwave frequency.............124
圖4.55 C-f and Loss-f performance of BZT(600℃ 500nm)/(Ta2O5)0.929(TiO2)0.071 (50nm)/HRS structure at Microwave frequency............. ..................................125
圖4.56 C-f and Loss-f performance of BZT(600℃ 500nm)/(Ta2O5)0.929(TiO2)0.071 (100nm)/HRS structure at Microwave frequency................................................126
圖4.57 C-f and Loss-f performance of BZT(600℃ 500nm)/(Ta2O5)0.929(TiO2)0.071 (200nm)/HRS structure at Microwave frequency................................................127
圖4.58 TEM Cross-section image of BZT(500nm 600℃)/Ta2O5(50nm)/HRS structure....... .............................128
圖4.59 TEM Cross-section image of BZT(500nm 600℃)/Ta2O5(100nm)/HRS structure....................................129
圖4.60 TEM Cross-section image of BZT(500nm 600℃)/Ta2O5(200nm)/HRS structure....................................130
圖4.61 C-V and Loss-V measurements of BZT(500nm 600℃)/Ta2O5(50 nm)/HRS structure....................................133
圖4.62 C-V and Loss-V measurements of BZT(600℃ 500nm)/(Ta2O5)0.929(TiO2)0.071 (50nm)/HRS................... ...132
圖4.63 C-V and Loss-V measurements of BZT(500nm 600℃)/Ta2O5(50 nm)/HRS structure annealed in N2 atmosphere..........133
圖4.64 C-V and Loss-V measurements of BZT(500℃ 500nm)/(Ta2O5)0.929(TiO2)0.071 (500nm)/HRS annealed in N2 atmosphere............................... ...............133
圖4.65 C-f and Loss-f of BZT/Ta2O5 (50nm)/HRS............135
圖4.66 C-f and Loss-f of BZT/(Ta2O5)0.929(TiO2)0.071 (50nm)/HRS...............................................136
圖4.67 Equivalent circuit of  BZT/buffer /HRS structure..137
圖4.68 Simulation structure in HFSS..................... 138
圖4.69 Simulated results of BZT(500nm)/HRS...............139
圖4.70 Simulated results of BZT(500nm)/buffer(50nm)/HRS..140

                                

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