利用快速升溫退火製備具[001]優選取向之序化鐵鉑薄膜與奈米粒子陣列之研究

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研究生：	王良瑋 Wang, Liang-Wei
論文名稱：	利用快速升溫退火製備具[001]優選取向之序化鐵鉑薄膜與奈米粒子陣列之研究 Achieving [001]-orientated films and nanoparticle arrays of L10-FePt via rapid thermal annealing
指導教授：	賴志煌
口試委員:	黃志青 Feng Yuan Ping 金重勳薛富盛唐敏注
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：	102
語文別：	英文
論文頁數：	139
中文關鍵詞：	鐵鉑、薄膜、奈米粒子、[001] 、垂直異向性、應力
外文關鍵詞：	FePt, film, nanoparticle, [001], perpendicular anisotropy, stress
相關次數：	點閱：1 下載：0
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幾年來，硬碟已成為一項相當重要的資訊儲存裝置。因其具備高儲存容量及低成本的特性，硬碟已被廣泛應用於電腦裝置及雲端儲存上。為了進一步提升硬碟碟片的記錄密度，開發新材料是一項極為重要的工作。序化鐵鉑合金被認為極有潛力成為下世代超高密度垂直記錄媒體之記錄材料，因此本論文針對鐵鉑合金之優選取向及微觀結構的控制進行研究。
第一部分探討如何藉由快速升溫退火的步驟提升序化鐵鉑合金之[001]優選取向。經由快速升溫退火，我們成功在400度的退火溫度下，於二氧化矽/矽基板上製備出具有高度[001]優選取向之序化鐵鉑合金。由於矽與鐵鉑合金在吸收紅外光的能力上有極大的差別，當快速升溫退火系統中的紅外光照到試片上時，矽會像吸光層一般吸收大量的光並提升其溫度，進而產生較大的熱膨脹量而使鐵鉑薄膜感受到一張應力。隨著升溫速率提升，快速升溫退火系統產生的瞬間光強度也愈強，使得鐵鉑合金感受到一較大的張應力，此張應力能有效促進序化鐵鉑合金[001]優選取向的生成。此外，此張應力亦能透過二氧化矽的性質進行調變。若二氧化矽的結構較鬆散，則張應力可能會於二氧化矽層中釋放掉，以致於無法得到較佳的[001]優選取向之序化鐵鉑合金。
第二部分則是研究從鐵鉑薄膜製備鐵鉑奈米粒子的方法，並試圖降低其製備溫度。透過臨場穿透式電子顯微鏡的觀察，我們發現隨著溫度升高，鐵鉑薄膜會經由孔洞成核與成長的過程，最後演變成奈米粒子。這些孔洞的成核與成長會沿著初鍍膜狀態之晶界進行。因為此微觀結構的變化是經由原子擴散進行，因此添加低熔點之氧化硼至鐵鉑薄膜中能使孔洞成核與成長所需的溫度降低。此外，加快原子擴散亦能促進鐵鉑合金之序化。在最佳化矽吸光層的厚度後，我們能夠使具[001]優選取向之序化鐵鉑合金的形成溫度由350度降低至250度，而鐵鉑奈米粒子的形成溫度亦能由700度下降至500度。
第三部分著重於利用具有有序表面形貌之基板以製備規則排列之鐵鉑奈米粒子陣列。基板之表面形貌是透過高分子之微觀相分離來製備，可以得到規則六角排列之碳氧化矽奈米球陣列，其平均直徑與球之中心間距分別為25及40奈米。藉由控制鐵鉑薄膜之厚度與奈米球之氧電漿處理時間，能夠在高溫退火後製備出六角規則排列之鐵鉑奈米粒子陣列，其直徑約20奈米，並且其排列是由碳氧化矽奈米球決定。在經過一氧化碳與氨氣電漿處理後，一些較微小的多餘奈米粒子能夠被移除，最後可以得到一個幾近完美六角排列之鐵鉑奈米粒子陣列。

Hard disk drives (HDDs) are very important devices for mass data storage, which are widely used in computer systems and cloud storage due to their low cost and high capacity. The development of new materials for recording disks is necessary to further increase the areal density in next-generation magnetic recording media. This dissertation focuses on three main research topics to manipulate the orientation and microstructure of FePt alloys that is a promising candidate as ultrahigh-density perpendicular magnetic recording media.
The first topic investigates promotion of the [001]-oriented L10-FePt by rapid thermal annealing (RTA) with a light absorption layer. By using RTA at 400 °C, the highly [001]-oriented L10-FePt grown on SiO2||Si is achieved. Due to the dramatic divergence of the light absorption ability between Si and FePt films, Si behaves as a light absorption layer to absorb much more light emitted from the RTA system, which gives rise to the larger thermal expansion on Si and induces an in-plane tensile stress on FePt films. By raising heating rate during RTA, the transient light intensity is increased; therefore, a higher in-plane tensile stress is exerted on FePt films, which effectively suppresses the opening-up in in-plane hysteresis loops. Furthermore, the (001) texture of the L10-FePt is manipulated by densities of the SiO2 underlayer. The in-plane tensile stress generated during RTA may be released in a loose SiO2 layer, which leads to the worse [001] orientation of the L10-FePt as compared to FePt films on a dense SiO2 layer.
The second topic aims at developing L10-FePt nanoparticles (NPs) by thermal dewetting at reduced temperatures. Through in situ heating transmission electron micro-scope (TEM) analysis, the mechanism of the formation process of the L10-FePt NPs is investigated, which demonstrates a typical thermal dewetting process, or called agglom-eration, via holes nucleation and growth. The holes are observed to nucleate and grow along the initial grain boundaries in as-deposited films. Because the evolution of the holes progresses via surface diffusion of atoms, the dewetting process is accelerated at reduced temperatures by adding B2O3 into FePt films due to the low melting point and high diffusivity of B2O3. The accelerated atomic diffusion also enhances the ordering of the L10-FePt. After optimizing thicknesses of the Si light absorption layer, annealing temperatures for the formation of the L10-FePt and FePt NPs can be dramatically decreased from 350 °C to 250 °C and from 700 °C to 500 °C, respectively.
The third topic focuses on fabricating periodic FePt NP arrays via templated dewetting of FePt films on a topographic template. Hexagonal-packed SiOC spheres with an average diameter of 25 nm and an average center-to-center distance of 40 nm are obtained on a flat thermally oxidized Si substrate through microphase separation of the PS-PDMS BCP to be used as the topographic templates for templated dewetting. By manipulating thicknesses of FePt films and O2 treatment time of the PS-PDMS BCP, well-ordered FePt NP arrays with a hexagonal packing are fabricated on top of the SiOC spheres. The size of the FePt NPs is around 20 nm that is well confined by the SiOC spheres and the location of these NPs is defined by the SiOC spheres because of their exactly equal center-to-center distances. After treated by Co/NH3 plasma to remove the excess small islands in between the SiOC spheres, a nearly perfect hexagonal-packed FePt nanoparticle array is obtained.

ABSTRACT    I
ABSTRACT (IN CHINESE)    V
TABLE OF CONTENTS    VII
LIST OF FIGURES    XI
LIST OF TABLES    XIX
LIST OF ABBREVIATIONS    XX
CHAPTER 1. INTRODUCTION    1
1 Motivation    2
2 Dissertation outline    5
CHAPTER 2. BACKGROUND    7
1 Properties of FePt    8
2 Uniaxial magnetic anisotropy    11
2.1. Magnetocrystalline anisotropy    12
2.2. Shape anisotropy    13
2.3. Magnetoelastic anisotropy    14
3 Reduction of ordering temperature for L10-FePt    16
3.1. Addition of third elements    16
3.2. Ion irradiation    17
3.3. Stress    17
4 Perpendicular magnetic anisotropy of L10-FePt    18
5 Thermal dewetting    20
5.1. Capillary Energies    22
5.2. Hole formation by thermal grooving    22
5.3. Templated dewetting    24
6 Block copolymers    28
6.1. Microphase separation    28
6.2. Applications to nanopatterning    30
CHAPTER 3. EXPERIMENTAL TECHNIQUES    33
1 Sample Fabrication    34
1.1. High Vacuum Sputtering System    34
1.2. Rapid thermal annealing    35
1.3. Reactive ion etching    36
2 Structure Characterization    37
2.1. X-Ray Diffractometer    37
2.2. Transmission Electron Microscope    38
2.3. Atomic Force Microscope    40
2.4. Fourier transform infrared spectroscopy    41
3 Magnetic Characterization    43
3.1. Vibrating Sample Magnetometer    43
3.2. Superconducting Quantum Interference Device    44
CHAPTER 4. PROMOTION OF [001]-ORIENTED L10-FEPT BY RAPID THERMAL ANNEALING    47
1 Introduction    47
2 Experimental Procedures    49
3 Results and discussion    50
3.1. Effect of stress on L10-FePt (001) ordering    50
3.2. Effect of Si thickness on L10-FePt (001) ordering    60
3.3. Effect of SiO2 underlayers on L10-FePt (001) ordering    65
4 Summary    71
CHAPTER 5. FABRICATION OF L10-FEPT NANOPARTICLES BY THERMAL DEWETTING    73
1 Introduction    73
2 Experimental Procedures    75
3 Results and discussion    77
3.1. FePt NPs by thermal dewetting    77
3.2. Morphology evolution during thermal dewetting    83
3.3. Effect of B2O3 on thermal dewetting and ordering of L10-FePt    93
4 Summary    99
CHAPTER 6. PERIODIC FEPT NANOPARTICLE ARRAYS ON TOPOGRAPHIC  SUBSTRATES    101
1 Introduction    101
2 Experimental Procedure    104
3 Results and discussion    107
3.1. Fabrication of SiOC sphere arrays    107
3.2. Hexagonal-packed FePt nanoparticle arrays on SiOC spheres    109
3.3. Morphology evolution of FePt films on SiOC spheres    119
3.4. Effect of RIE treatment on FePt nanoparticle arrays    122
4 Summary    124
CHAPTER 7. CONCLUSIONS    125
REFERENCES    129

                                

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