中文摘要：
近年來，超大型積體電路採用高介電材料取代二氧化矽做為動態記憶體中電容之介電材料日趨明顯。隨著高密度動態記憶體中電荷儲存結構尺寸之縮減，二氧化鈦與鈦酸鋇由於具有高介電常數、高折射係數和高化學穩定性，故有希望應用於高密度動態記憶體之介電材料。本論文旨在研發高介電二氧化鈦(TiO2)薄膜與鈦酸鋇(BaTiO3, BTO)薄膜的沉積方法與薄膜特性之研究。二氧化鈦與鈦酸鋇具有較高的介電常數(εr)，因此可以被運用在動態隨機存取記憶體(DRAM)或電子元件中之絕緣層。但由於傳統成長氧化層的方法，如：分子束磊晶(MBE)化學氣相沉積(CVD)均須在高溫沉積，高溫會對元件造成一定程度的傷害。所以我們研究一種新的技術 “以液相沉積法(Liquid Phase Deposition-LPD) 生長鈦酸鋇(BaTiO3)薄膜”，其過程簡單、成本低廉、而且成長溫度極低(小於100℃)，因此值得廣泛研究和發展。對於測量此法所得的鈦酸鋇薄膜特性方面，我們利用掃描式電子顯微鏡(SEM) 、二次離子質譜儀(SIMS) 、傅立葉紅外線光譜儀(FTIR)與歐傑電子光譜儀(AES)分析，可得到鋇、鈦、氧的組成縱深分佈。另外，由漏電流密度-電場強度曲線(J-E Curve)與電容-電壓曲線(C-V Curve)我們可瞭解兩薄膜的漏電效應並得知平帶電壓偏移(VFB) 、介電常數(εr)與有效電荷密度(Qeff)。此外，我們使用熱退火與熱氧化來改善二氧化鈦薄膜與鈦酸鋇薄膜的漏電流特性。二氧化鈦薄膜與鈦酸鋇薄膜介電常數分別可高達40與62，漏電流亦可分別降低至1 × 10-5 A/cm2與5 × 10-9 A/cm2。
未來改進的目標 (1)提高兩薄膜內的氧成份比，以及提升鈦酸鋇薄膜內的鋇含量。(2)研發更簡易的原料配製過程。(3)對所提沉積機制的在檢驗。

ABSTRACT

In recent years, there has been increasing demands for high dielectric materials to replace SiO2 for high-density dynamic random access memories with ultra large scale integration (ULSI). As the dimensions of the charge storage node decrease in high-density dynamic random access memories (DRAMs), TiO2 and BaTiO3 are very promising candidates for applications with exhibiting higher dielectric constant, high refractive index and high chemical stability.
The physical and chemical properties of LPD thin film by means of several measuring instruments, including Fourier Transform Infrared Spectrometer (FTIR), Auger Electron Spectroscopy (AES), Secondary Ion Spectrometer (SIMS), and X-Ray Diffractometer (XRD). As for the category in the electrical properties, such as C-V curve and I-V curve, of LPD-BTO thin film is comprehended in the most important part of this chapter. Further, we try to improve these electrical properties of LPD-TiO2 and LPD-BTO thin film by post-annealing in oxygen atmosphere at several high temperatures.
From leakage current density-electric field intensity voltage (J-E) and capacitance-voltage (C-V) measurements, the leakage current densities are about (LPD-TiO2: 1 × 10-5 A/cm2 and LPD-BTO: 5 × 10-9 A/cm2). And the individual dielectric constants of both films (TiO2 and BTO) are calculated about 40 and 60. This value is larger than thermal oxide, PECVD oxide, and LPD-SiO2. We also can obtain the flat band voltage shifts of LPD-TiO2 and LPD-BTO films which are about –0.5V and 0V; the effective oxide charges which are calculated about –4.52×1011 cm-2 and –2.27×1012 cm-2
The future goals:
(1) Raising the atomic concentration of oxygen within both films and of barium within LPD-BTO film.
(2) Shortening the process in preparation of both deposition solutions.
(3) Re-checking both models.

CONTENTS

LIST OF FIGURES……………………………………………………...I
LIST OF TABLES………………………………………………………V ABATRACT…………………………………………………………… VI

1.INTRODUCTION……………………………………………………...1
1-1 Trend in DRAM Dielectrics………………………………………1
1-2 High Dielectric Constant Material
Barium Titanate (BaTiO3)……………………………………2
1-3 Background of Liquid Phase Deposition (LPD) in Our Lab……...4
1-3-1 LPD-SiO2 …………………………………………………...4
1-3-2 LPD-SiON and Biased-LPD-SiON…………………………6
1-3-3 LPD-TiO2 and LPD-BTO…………………………………...7
1-4 Advantages of LPD Deposition1………………………………...11

2.EXPERIMENTS………………………………………………………13
2-1 Deposition System………………………………………………13
2-2 Cleaning of Silicon Substrate……………………………………14
2-3 Preparation of Deposition Solution……………………………...15
2-3-1 Preparation of Precursors…………………………………..15
2-3-2 Preparation of LPD-TiO2 Deposition Solution…………….17
2-3-3 Preparation of LPD-BTO Deposition Solution…………….19
2-3-4 Difference between LPD-TiO2 and LPD-BTO Deposition Soluiotns…………………………………………………..20
2-4 Film Deposition………………………………………………….21
2-5 Characteristics…………………………………………………...22
2-5-1 Physical Properties………………………………………...22
2-5-2 Chemical Properties………………………………………..22
2-5-3 Electrical Properties – MOS Structure…………………….23

3.RESULTS AND DISCUSSION………………………………………26

PART A: Investigation of LPD-TiO2 Films on Silicon Substrate………27
3-1 Mechanisms of LPD-TiO2 Deposition…………………………..27
3-1-1 Crystallinity of LPD-TiO2 Film……………………………27
3-1-2 Model of LPD-TiO2 Deposition…………………………...27
3-1-3 Chemical Equilibrium of LPD-TiO2 Deposition…………..29
3-2 Deposition Parameters and Physical Properties of LPD-TiO2
Films…………………………………………………………...31
3-2-1 Deposition Rate and Refractive Index as a Function of
Deposition Time…………………………………………...31
3-2-2 Deposition Rate and Refractive Index as a Function of
Deposition Temperature………………..…………..……...33
3-2-3 Deposition Rate and Refractive Index as a Function of
H3BO3 Molarity in the Deposition Solution……………….34
3-3 Chemical Properties of As-deposited LPD-TiO2 Films…………35
3-3-1 AES Depth Profile of LPD-TiO2 Film……………………..36
3-3-2 SEM View of LPD-TiO2 Films…………………………….36
3-3-3 SIMS Depth Profile of As-deposited LPD-TiO2 Film……..37
3-3-4 Analyses of Room Temperature FTIR Spectra ……………37
3-4 Electrical Characteristics of As-deposited LPD-TiO2 Film……..39
3-4-1 J-E Measurement…………………………………………..39
3-4-2 C-V Measurement………………………………………….40

PART B: Investigation of LPD-BTO Thin Films on Silicon Substrate...42
3-5 Mechanisms of LPD-BTO Deposition…………………………..42
3-5-1 Crystallinity of LPD-BTO Thin Film……………………...42
3-5-2 Model of LPD-BTO Deposition…………………………...42
3-5-3 Chemical Equilibrium of LPD-BTO Deposition…………..43
3-6 Deposition Parameters and Physical Properties of LPD-BTO Films…………………………………………………………….45
3-6-1 Deposition Rate and Refractive Index as a Function of
Deposition Time…………………………………………...45
3-6-2 LPD-BTO Thin-Film Deposition in Initial Period………...46
3-6-3 Deposition Rate and Refractive Index as a Function of
Deposition Temperature…………………………………...47
3-6-4 Deposition Rate and Refractive Index as a Function of
H3BO3 Molarity in the Deposition Solution……………….49
3-7 Chemical Properties of As-deposited LPD-BTO Films…………50
3-7-1 AES Depth Profile and Survey Scan of LPD-BTO Film….50
3-7-2 SEM View of LPD-BTO Films……………………………51
3-7-3 SIMS Depth Profile of As-deposited LPD-BTO Film…….51
3-7-4 Analyses of Room Temperature FTIR Spectra…………….52
3-8 Electrical Characteristics of As-deposited LPD-BTO Film……..52
3-8-1 J-E Measurement…………………………………………..52
3-8-2 C-V Measurement………………………………………….53
3-8-3 Leakage Current Mechanisms……………………………..53
3-9 Improvements of Leakage Current by Annealing in Oxygen Ambient…………………………………………………………..54

4. CONCLUSIONS………………………………………………….58

FIGURES………………………………………………………60~100
TABLES………………………………………………………101~103
REFERENCES………………………………………………..104~110

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