新式相變化材料開發與改質｜國立清華大學博碩士論文庫

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研究生：	張博欽 Chang, Po-Chin
論文名稱：	新式相變化材料開發與改質 Development and Modifications of Novel Phase-change Materials
指導教授：	張士欽 Chang, Shih-Chin 金重勳 Chin, Tsung-Shune
口試委員:	張士欽 Chang, Shih-Chin 金重勳 Chin, Tsung-Shune 謝宗雍 Hsieh, Tsung-Eong 何永鈞 Her, Yung-Chiun 陳貞光 Chen, Jhewn-Kuang
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：	2013
畢業學年度：	101
語文別：	英文
論文頁數：	164
中文關鍵詞：	相變化記憶體、結晶動力學、多階儲存、相變化材料
外文關鍵詞：	Phase-change memory, Crystallization Kinetics, Multi-level memory, Phase-change materials
相關次數：	點閱：2 下載：0
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相變記憶體是先進非揮發性記憶體中重要的一員。本論文探討摻雜異質元素對相變化材料的影響及評估新穎材料在相變化記憶體的應用。從具有優異熱穩定性的三元鎵銻碲合金出發，利用添加矽進行改質，成功開發出具超高熱穩定性的四元相變化材料。結晶行為屬成長控制型的二元鎵銻合金雖有相分離的潛在缺點，但可被用於多階儲存用途。此二元鎵銻合金更進一步利用矽進行改質，發現其仍具有高速操作特性，同時熱穩定性大幅被提升。最後評估具有共晶組成的鍺鋁二元合金以及全固相相轉變的共析鋼用於相變化記憶體的可行性。
第一主題為鎵銻碲三元合金薄膜開發，包含熱性質、結晶構造、結晶動力學等基礎物性研究，並進行記憶體元件的電性測試。鎵銻碲薄膜展現出高度熱穩定性的高結晶溫度(Tx: 253 °C)及高結晶活化能(Ea: 5.8 eV)，非晶薄膜更可在201 °C下保存長達10年以上時間。薄膜具有單相結晶結構，結晶化過程具有9 %的體積收縮率。其記憶體元件可以在10奈秒的電壓脈衝進行寫入/擦拭的動作，在優化的操作條件下可循環操作超過109次。
第二主題為矽添加鎵銻碲四元合金薄膜的開發，其中組成為Si29(Ga2TeSb7)71的合金具有非常優異的熱穩定性，結晶溫度達340 °C，10年資料保存溫度為254 °C。利用此組成製成的元件其高阻狀態可承受超過25分鐘的250 °C恆溫加熱。非晶化過程可以在10奈秒完成，唯結晶化過程需要20微秒，此結果與我們利用結晶動力學預測的結果相符。元件可以重複進行寫入/擦寫動作超過106次。化學電子能譜儀分析顯示當矽含量超過10 at.%會形成矽碲鍵結。利用化學電子能譜儀分析的鍵結型式，我們可以較為準確的預測薄膜的結晶溫度以及玻璃轉換溫度。
第三主題為以二元鎵銻合金為基底，利用矽進行改質。Ga19Sb81合金具有合適的熱穩定性，其結晶溫度為228 °C，十年資料保存溫度為156 °C。元件測試結果現顯示Ga19Sb81合金可於10至100奈秒內完成寫入/擦寫的動作。更重要的發現為其具有多階儲存的能力。矽添加後的Ga19Sb81合金熱穩定性依矽含量有著顯著的提升，結晶溫度為236至284 °C，十年資料保存溫度為 171至217 °C。加Si 4 at.%的組成可於40奈秒內完成寫擦動作，而添加9 at.% Si的合金為100奈秒。耐久度測試以組成S9為最佳，目前可達104次。
第四主題探討共晶合金以及共析鋼於相變記憶體的應用。鍺鋁共晶合金可分別於10奈秒及80奈秒完成寫擦動作，耐久度測試達104次。鎳添加共析鋼可於10奈秒完成寫擦，耐久度達105次。其他共晶系合金諸如矽基以及銻基也被提出，這些共晶系合金具有與目前半導體製程相容的利基。共析合金具有全固相相變機制，可以藉此提升元件的可靠度。

Phase-change random access memory (PCRAM) is one of the most important emerging non-volatile memories. The purpose of this dissertation is to study the effect of modification on new phase-change materials for applications in PCRAM. We worked out Ga-Te-Sb and Si-doped Ga-Te-Sb alloys for highly thermal stable PCRAM and Ga-Sb for multi-level storage applications. Meanwhile, Si-doped Ga-Sb alloys are suitable for high-speed operation while retain excellent thermal stability. Eutectic Ge-Al alloy for PCRAM was also evaluated. Finally, solid-state phase transformation based on Fe-C alloy is proposed.
The Ga2TeSb7 films exhibit a high crystallization temperature (Tx: 253 °C), high temperature corresponding to 10-year data retention (T10y: 201 °C) and high activation energy of crystallization (Ea: 5.76 eV) hence providing outstanding thermal stability. X-ray diffraction (XRD) analysis showed that amorphous Ga2TeSb7 crystallizes into single R3m Sb-structure. The density change of Ga2TeSb7 film is 8.9 %, which is smaller than GST (9.5 %). Ga2TeSb7 memory cells demonstrate fast SET/RESET operation within 10 ns and excellent cycling endurance up to 109 cycles.
Si-doped Ga2TeSb7, Si29(Ga2TeSb7)71, showed further improved thermal stability (Tx: 340 °C, T10y: 254 °C, Ea: 5.2 eV). Data retention of Si29(Ga2TeSb7)71 memory cells is beyond 1500 s at 250 °C. The memory cell can be operated using set and reset pulses at 20 μs and 10 ns, respectively, over 106 cycles. X-ray photoelectron spectroscopy (XPS) results showed the formation of Si-Te bonds as Si content is greater than 10 at.%. Based on bonding status revealed by XPS, prediction of glass-transition temperature (Tg) and Tx can thus be more dependable.
Tx, T10y and Ea of Ga19Sb81 thin films are 228 °C, 156 °C and 4.7 eV, respectively. Ga19Sb81 memory cell can be operated within 10-100 ns. Most importantly, it shows multi-level capability (3 bits/cell). Tx, T10y and Ea of Si-doped Ga19Sb81 films (Si at.% : 1~14) are 236-284 °C, 171-217 °C and 5.3-9.1 eV, respectively. The memory cells of Si4(Ga19Sb81)96 film show reversible switching within 40-200 ns and that of Si9(Ga19Sb81)91 film is 100 ns. The endurance for Si4(Ga19Sb81)96 and Si9(Ga19Sb81)91 memory cells are ~103 and 104, respectively. All of our developed materials showed remarkable thermal stability than the benchmark material Ge2Sb2Te5 (Tx: 176 °C, T10y: 93 °C, Ea: 3.1 eV) while having satisfactory operation speed. They have the chance to replace NOR Flash even the DRAM technology.
Ge-Al film with eutectic composition can be set and reset in 10 ns and 80 ns, respectively. Cycling times can be up to 104. Fe-Ni-C film can be set and rest within 10 ns while showing reversible switching over 105. Others such as Si-based and Sb-based films also show potential applications in PCRAM.

Abstract    I
摘要    II
誌謝    III
Table of Content    IV
List of Tables    VIII
List of Figures    X
CHAPTER 1 Background and Motivations    1
1 Introduction to Memory Technologies    1
1.1 Volatile memory technologies    1
1.2 The NVM technologies    2
1.3 Emerging NVM technologies    4
2 Motivations    8
2.1 History of PCRAM    8
2.2 Potential applications of PCRAM    10
2.3 Challenges of PCRAM    12
3 Objectives of This Study    15
3.1 Modification of Ga2TeSb7 for high thermal stability PCRAM    16
3.2 Ga19Sb81 for multi-level storage application    17
3.3 Modification of Ga19Sb81 for high thermal stability and high speed applications    17
3.4 Exploring binary eutectic phase-change materials    17
3.5 Exploring solid state transformation phase-change materials    18
CHAPTER 2 Literature Review on Phase-change Memory    19
1 Status of PCRAM    19
1.1 Properties of phase-change materials    19
1.2 Device structures    31
1.3 Reliability of PCRAM    34
2 Novel Phase-change Materials    36
2.1 Modification of the benchmark material Ge2Sb2Te5    37
2.2 Unary phase-change material    38
2.3 Binary phase-change materials and their modifications (Ge-based, Sb-based, Te-based)    39
2.4 Ternary phase-change materials    41
3 Crystallization Kinetics of Phase-change Materials    41
3.1 Theory of non-isothermal crystallization process    41
3.2 Isothermal kinetic analysis    43
4 Estimating Crystallization Properties by Calculations    43
CHAPTER 3 Experimental Procedures    45
1 Experiments on Phase-change Films    45
1.1 Sample preparation and measurements    45
1.2 Procedures of kinetic analysis of phase-change films    46
2 Fabrication of Memory Test-cells and Cell-testing    48
CHAPTER 4 Phase-change Materials Based on Modified Ga2TeSb7    51
1 Study of Ga2TeSb7    51
1.1 The properties of Ga2TeSb7 films    51
1.2 The crystallization kinetics of Ga2TeSb7 film    58
1.3 The performance of devices based on Ga2TeSb7    61
2 Study of N-doped Ga2TeSb7    62
2.1 The properties of N-added Ga2TeSb7 films    62
3 Study of Si-doped Ga2TeSb7    64
3.1 The properties of Si-added Ga2TeSb7 films    64
3.2 The crystallization kinetics of Si-doped Ga2TeSb7 films    71
3.3 The estimation of Tg and Tx    80
3.4 The performance of devices based on Si-doped Ga2TeSb7    82
4 Study of Ge-doped Ga2TeSb7    83
4.1 The properties of Ge-added Ga2TeSb7 films    83
4.2 The crystallization kinetics of Ge-doped Ga2TeSb7 films    85
5 Summary    91
CHAPTER 5 Phase-change Materials Based on Modified Ga19Sb81    92
1 Study of Ga19Sb81    92
1.1 The properties of Ga19Sb81 films    92
1.2 The performance of devices based on Ga19Sb81    97
2 Study of Si-doped Ga19Sb81    101
2.1 The properties of Si-doped Ga19Sb81 films    102
2.2 The crystallization kinetics of Si-added Ga19Sb81 films    106
2.3 The performance of devices based on Si-added Ga19Sb81    116
3 Summary    117
CHAPTER 6 Exploration of Advanced Phase-change Materials    119
1 Study of Ge Based Eutectic Alloys    119
1.1 Preliminary surveying of new materials    119
1.2 The performance of devices based on eutectic Ge-Al    127
2 Study of Si Based Eutectic Alloys    129
3 Study of Sb Based Eutectic Alloys    131
4 Study of Fe-C films    133
4.1 The performance of devices based on Fe-C    134
4.2 Comparison of phase-change memories made of Fe-C and Ga-Sb    138
CHAPTER 7 Conclusions and Suggestion for Future Works    140
1 Conclusions of This Study    140
2 Suggestions for Future Works    142
References    144
Publication list    164


                                

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