利用反應式射頻磁控濺鍍法鍍製二氧化釕薄膜之分析

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研究生：	陳俊宇 Chun-yu Chen
論文名稱：	利用反應式射頻磁控濺鍍法鍍製二氧化釕薄膜之分析 The Characterization of Textured Ruthenium Dioxide (RuO2) Thin Films Prepared with Reactive RF Magnetron Sputtering
指導教授：	甘炯耀 Jon-yiew Gan
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：	2004
畢業學年度：	92
語文別：	英文
論文頁數：	75
中文關鍵詞：	二氧化釕、射頻磁控濺鍍、X光光電子能譜儀
外文關鍵詞：	RuO2, RF Magnetron Sputtering, XPS
相關次數：	點閱：2 下載：0
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本研究主要是著重在利用反應式射頻磁控濺鍍法鍍製二氧化釕薄膜之指向控制與分析。
改變濺鍍時的參數，包括氧氣流量比例、基板溫度、工作壓力、瓦數及基板種類，並分別利用X光繞射儀、掃瞄式電子顯微鏡、掃瞄探針顯微鏡及X光光電子能譜儀觀察參數改變對二氧化釕薄膜之指向、表面型態、表面粗糙度及化學鍵結的影響。
在氧氣流量比例為30%、基板溫度為300℃的環境之下，我們可以製備出具(110)優選指向的二氧化釕薄膜。而具備(101)優選指向的二氧化釕薄膜則是在高氧流量比例(50%)及高基板溫度(450℃)的環境下成長。二氧化釕薄膜表面粗糙度會隨著氧氣流量比例和基板溫度的上升而增加。在低氧氣流量比時，薄膜表片化學鍵結主要是由金屬釕與二氧化釕所組成。隨著氧氣的流量比增加，三氧化釕的鍵結便逐漸形成，而且比例會隨著氧氣流量比例與基板溫度的上升而增加。
將基板種類由二氧化矽改成釕金屬/二氧化矽基板及白金/氧化鎂單晶基板，則二氧化釕薄膜呈現(200)優選指向，不受氧氣流量比、基板溫度及表面化學鍵結的影響。

The research is concentrated in the orientation control and characterization of ruthenium dioxide (RuO2) thin films deposited by RF magnetron sputtering.
Changing sputtering parameters, including O2 flow ratio, substrate temperature, RF power density, and substrate type, is investigated. And the effects of sputtering parameters on the orientation, surface morphology, surface roughness, and chemical bonding of RuO2 thin films are characterized by XRD, SEM, SPM, and XPS respectively.
Under mediate O2 flow ratio (25%) and lower substrate temperature (300℃), we get the (110)-orientation preferred RuO2 films, and the (101)-orientation preferred films growth under high O2 flow ratio (50%) and high substrate temperature (450℃). The surface becomes rougher with the increase of O2 flow ratio and substrate temperature. The chemical bonding exhibits the coexistence of Ru and RuO2 under lower O2 flow ratio. As O2 flow ratio is raised, RuO3 is found in XPS spectra, and the ratio will increase with the O2 flow ratio and substrate temperature. Besides, by changing substrate as Ru or Pt/MgO, the RuO2 films will exhibit highly (200)-oriented films, no matter the O2 flow ratio, substrate temperature, and chemical bonding.

List of Contents
Abstract    Ⅰ
Acknowledgements    Ⅱ
List of Contents    Ⅳ
List of Tables    Ⅵ
List of Fugures    Ⅶ
Chapter 1.  Introduction    1
Chapter 2. Literature Review    3
2-1. Physical properties of RuO2    3
2-2. Application of RuO2    4
2-3. Control of RuO2 Orientation    7
Chapter 3. Experimental    15
3-1. Prepare of RuO2 thin films    15
3-1-1. Prepare and clean procedures of SiO2/Si substrates 15
3-1-2. Prepare of RuO2 on Ru/SiO2/Si substrates           16
3-1-3. Preparation of RuO2 thin film on Pt/MgO substrates 16
3-1-4. Preparation of RuO2 thin films on SiO2/Si substrates 17
3-2. Characterization of RuO2 thin films    17
Chapter 4 Results and Discussion    24
4-1. Orientations of deposited RuO2 thin films    24
4-2. Surface morphology of textured RuO2 thin films    27
4-3. Quantitative chemical analysis of RuO2 thin films    30
4-4. Discussion    34
Chapter 5 Conclusions    67
Reference    68
List of Tables
Table 3-1    The parameters of Ru/RuO2 multi-layer deposition
(a)Ru (b) RuO2    19
Table 3-2    The parameters of RuO2 thin films deposited on Pt/MgO substrates    20
Table 3-3    The parameters of RuO2 thin films deposited on SiO2/Si substrates    20
Table 4-1    The binding energy of ruthenium oxide thin films as obtained from a least-square curve fitting procedure of experimental XPS data    40
Table 4-2    The area ratio of XPS peak for RuO2 thin films deposited under different O2 flow ratio. The substrate temperature is fixed at 300℃.    40
Table 4-3    The area ratio of XPS peak for RuO2 thin films deposited under different substrate temperature. The O2 flow ratio is fixed at 50%    41
Table 4-4    The area ratio of XPS peak for RuO2 thin films depos-
ited on Pt/MgO substrates under different O2 flow ratio.
The substrate temperature is fixed at 450℃.    41
List of Figures
Figure 2-1    The rutile structure unit cell    9
Figure 2-2    Density of states for the valence (oxygen p levels) and conduction (metal d level) band of RuO2    9
Figure 2-3    The effect of fatigue on P-E curve    10
Figure 2-4    Fatigue properties of (a) RuO2 /PZT/Pt/RuO2 capacitor (b) Pt/PZT/Pt capacitor fabricated using PZT films deposited at 395℃    10
Figure 2-5    Schematic diagrams of supposed lattice matching image    11
Figure 2-6    XRD curves of the (Bi3.5Nd0.5)Ti3O12 films deposited on (a) (101)RuO2//(012)Al2O3 and (b) (001)RuO2 // (001)TiO2 substrates    11
Figure 2-7    XRD spectra of as-deposited RuO2 films deposited at a relative O2 partial pressure of 20% and 50%; sputtering power was 0.2 kW at 12 mTorr. No intentional substrate heating was applied during the deposition    12
Figure 2-8    XRD patterns of RuO2 films prepared at various substrate temperatures (a) 25℃ (b) 100℃ (c) 200℃ (d) 300℃ (e) 400℃ (f) 500℃. The films were deposited for 1h at gas flow ratio of 70/30, the working pressure of 0.66Pa, and the RF power of 80W    12
Figure 2-9    XRD patterns of RuO2 films deposited at various O2 content of the working gas (a) 10% (b) 20% (c) 30% (d) 40%. The films deposited for 1h at the substrate temperature of 500℃, the working pressure of 0.66Pa, and the RF power of 80W    13
Figure 2-10    XRD pattern of a PZT thin film grown on a RuO2/MgO substrate    13
Figure 2-11    XRD patterns of RuO2/Ru multilayers deposited on
SiO2/Si substrates    14
Figure 2-12    XRD patterns of RuO2 films on Pt(111), Ru(001),
and TiO2    14
Figure 3-1    The diagram of the RF magnetron sputter system    21
Figure 3-2    RuO2 thin films deposition and characterization    22
Figure 3-3 (a)    The structure of RuO2/Ru/SiO2/Si substrate    23
Figure 3-3 (b)    The structure of the RuO2/Pt/Mgo substrate    23
Figure 3-3 (c)    The RuO2/ SiO2/Si structure    23
Figure 4-1    The XRD patterns of RuO2 films deposited on SiO2
with O2 flow ratio = (a) 15% (b) 20% (c) 25% (d)
30% (e) 50%. The Ts = 300℃, working pressure
= 10 mTorr, and the RF power = 20W    42
Figure 4-2    The XRD patterns of RuO2 films deposited on SiO2
with O2 flow ratio = (a) 15% (b) 30% (c) 40% (d)
50%. The Ts = 450℃, working pressure = 10 mTorr,
and the RF power = 20W    43
Figure 4-3    The XRD patterns of RuO2 films deposited on SiO2
with O2 flow ratio = (a) 15% (b) 20% (c) 30% (d)
50%. The Ts = 300℃, working pressure = 5 mTorr,
and the RF power = 20W    44
Figure 4-4    The XRD patterns of RuO2 films deposited on SiO2
with O2 flow ratio = (a) 15% (b) 30% (c) 40% (d)
50%. The Ts = 450℃, working pressure = 5 mTorr,
and the RF power = 20W    45
Figure 4-5    The effect of RF power density on the crystallization
of (200)-oriented RuO2 films    46
Figure 4-6    The XRD curve of RuO2 films deposited on Ru at Ts
= (a) 200℃ (b) 100℃. The O2 flow ratio = 30%,
working pressure = 5 mTorr,  RF power = 20W    47
Figure 4-7    The XRD curves of RuO2 films deposited on
Pt/MgO with O2 flow ratio = (a) 15% (b) 30% (c)
40%. The Ts = 450℃, working pressure = 5 mTorr,
RF power = 20W    48
Figure 4-8    The SEM images of (110)-orientation preferred
RuO2 films deposited on SiO2 with O2 flow ratio =
(a) 25% (b) 30%. The Ts = 300℃, working pressure
= 10 mTorr, and the RF power = 20W    49
Figure 4-9    The AFM images of (110)-orientation preferred
RuO2 films deposited on SiO2 with O2 flow ratio =
(a)    25% (b) 30%. The Ts = 300℃, working pressure
= 10 mTorr, and the RF power = 20W    50
Figure 4-10    The SEM images of (101)-orientation preferred
RuO2 films deposited on SiO2 with O2 flow ratio =
(a)    40% (b) 50%. The Ts = 450℃, working pressure
= 10 mTorr, and the RF power = 20W    51
Figure 4-11    The AFM images of (101)-orientation preferred
RuO2 films deposited on SiO2 with O2 flow ratio =
(a)    40% (b) 50%. The Ts = 450℃, working pressure
= 10 mTorr, and the RF power = 20W    52
Figure 4-12    The (a) SEM (b) AFM images of RuO2 films
deposited on Ru at Ts = 200℃, O2 flow ratio = 30%,
working pressure = 5 mTorr,  RF power = 20W    53
Figure 4-13    The GIXD patterns of RuO2 films deposited on Ru at Ts = 200℃, O2 flow ratio = 30%, working pressure = 5 mTorr,  RF power = 20W    54
Figure 4-14    The (a) SEM (b) AFM images of RuO2 films deposited on Pt/MgO at Ts = 450℃, O2 flow ratio = 40%, working pressure = 5 mTorr, and the RF power = 20W    55
Figure 4-15    The XPS spectra (a) Ru 3d (b) O1s peaks of RuO2 films deposited on SiO2 with O2 flow ratio = 15%, Ts = 300℃, working pressure = 10 mTorr, and the RF power = 20W    56
Figure 4-16    The XPS spectra (a) Ru 3d (b) O1s peaks of RuO2 films deposited on SiO2 with O2 flow ratio = 25%, Ts = 300℃, working pressure = 10 mTorr, and the RF power = 20W    57
Figure 4-17    The XPS spectra (a) Ru 3d (b) O1s peaks of RuO2 films deposited on SiO2 with O2 flow ratio = 30%, Ts = 300℃, working pressure = 10 mTorr, and the RF power = 20W    58
Figure 4-18    The XPS spectra (a) Ru 3d (b) O1s peaks of RuO2 films deposited on SiO2 with O2 flow ratio = 50%, Ts = 300℃, working pressure = 10 mTorr, and the RF power = 20W    59
Figure 4-19    The XPS spectra (a) Ru 3d (b) O1s peaks of RuO2 films deposited on SiO2 with O2 flow ratio = 50%, Ts = 400℃, working pressure = 10 mTorr, and the RF power = 20W    60
Figure 4-20    The XPS spectra (a) Ru 3d (b) O1s peaks of RuO2 films deposited on SiO2 with O2 flow ratio = 50%, Ts = 450℃, working pressure = 10 mTorr, and the RF power = 20W    61
Figure 4-21    The XPS spectra (a) Ru 3d (b) O1s peaks of RuO2 films deposited on Pt/MgO substrates with O2 flow ratio = 15%, Ts = 450℃, working pressure = 5 mTorr, and the RF power = 20W    62
Figure 4-22    The XPS spectra (a) Ru 3d (b) O1s peaks of RuO2 films deposited on Pt/MgO substrates with O2 flow ratio = 40%, Ts = 450℃, working pressure = 5 mTorr, and the RF power = 20W    63
Figure 4-23    The reaction process models of the RuO2 films growth by reactive sputtering under (a) low O2/Ar (b) mediate O2/Ar (c) high O2/Ar ratio    64
Figure 4-24    Two-dimensional atomic configurations of Ru and RuO2: (a) Ru (001) p plane (b) RuO2 (100) plane (c) epitaxial relationship between 5×4 Ru (001) and 3 × 3 RuO2 (100) planes    65
Figure 4-25    Probable epitaxial relationships of rutile on Pt    65
Figure 4-26    The 1-D growth of bar-like grains for (101)-oriented RuO2 films    66

                                

Chapter 1
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Chapter 2
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[8] T. Watanabe, T. Kojima, H. Uchida, I. Okada, and H. Funakubo, “Spontaneous Polarization of Neodymium-Substituted Bi4Ti3O12 Estimated from Epitaxially Grown Thin Films with in-Plane c-Axis Orientations”, Jpn. J. Appl. Phys., Vol. 43, No. 2B, pp L309-L311 (2004)
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[11] J. Zhai and H. Chen, “Ferroelectric properties of Bi3.25La0.75Ti3O12 thin films grown on the highly oriented LaNiO3 buffered Pt/Ti/SiO2 ’Si substrates”, Appl. Phys. Lett., Vol. 82, No. 3, pp.442-444 (2003)
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[17] B. H. Park, B.S Kang, S. D. Bu, T. W. Noh, J. Lee, and W. Jo, “Lanthanum-substituted Bismuth Titanate for Use in Non-volatile Memories”, Nature, Vol. 401, pp. 682-684 (1999)
[18] J. F. Scott, “Quantitative measurement of space-charge effects in lead zirconate-titanate memories”, J. Appl. Phys., Vol. 70, No. 1, pp. 382-388 (1991)
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[20] R. Ramesh, W. K. Chan, B. Wilkens, H. Gilchrist, T. Sands, J. M. Tarascon, V. G. Keramidas, D. K. Fork, J. Lee, and A. Safari, “Fatigue and Retention in Ferroelectric Y-Ba-Cu-O/Pb-Zr-Ti-O/Y-Ba-Cu-O Heterostructures”, App. Phys. Lett., Vol. 61, No, 13, pp. 1537-1539 (1992)
[21] C. B. Eom, R. B. Van Dover, Julia M. Phillips, D. J. Werder, J. H. Marshall, C. H. Chen, R. J. Cava, R. M. Fleming, and D. K. Fork, “Fabrication and properties of epitaxial ferroelectric heterostructures with (SrRuO3) isotropic metallic oxide electrodes”, Appl. Phys. Lett., Vol. 63, No. 18, pp.2570-2572 (1993)
[22] M. S. Chen, T. B. Wu, and J. M. Wu, “Effect of textured LaNiO3 electrode on the fatigue improvement of Pb(Zr0.53Ti0.47)O3 thin films”, Appl. Phys. Lett., Vol. 68, No. 10, pp. 1430-1432 (1996)
[23] X. Fang, M. Tachiki, and T. Kobayashi, “Growth of RuO2 Thin Films on a MgO Substrate by Pulsed Laser Deposition Method”, Jpn. J. Appl. Phys., Vol. 36, Part 2, No. 4B, pp. L511-514 (1997)
[24] J. F. Tressler, K. Watanabe, and M. Tanaka, “Synthesis of Ruthenium Dioxide Thin Film by a Solution Chemistry Technique”, J. Am. Ceram. Soc., Vol. 79, No. 2, pp. 525-529 (1996)
[25] S. Bhaskar, P. S. Dobal, S. B. Majumder, and R. S. Katiyar, “X-Ray Photoelectron Spectroscopy and Micro-Raman Analysis of Conductive RuO2 thin Films”, J. Appl. Phys., Vol. 89, No. 5, pp. 2987-2992 (2001)
[26] W. T. Lim, K. R. Cho, and C. H. Lee, “Structural and Electrical Properties of RF-sputtered RuO2 Films Having Different Conditions of Preparation”, Thin Solid Films, Vol. 348, No. 1, pp. 56-62 (1999)
[27] J. G. Lee, Y. T. Kim, and S. K Min and S. H. Choh, “Effects of excess oxygen on the properties of reactively sputtered RuOx thin films”, J. Appl. Phys. Vol. 77, No. 10, pp.5473-5475 (1995)
[28] Y. Kaga, Y. Abe, H. Yanagisawa, K. Sasaki, “Formation Process and Electrical Property of RuO2 Thin Films Prepared by Reactive Sputtering”, Jpn. J. Appl. Phys. Vol. 37, Part 1, No. 6A , pp. 3457-3461 (1998)
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Chapter 4
[1] Y. Abe., M. Kawamura and K. Sasaki, “Highly Textured (100) RuO2/(001) Ru Multilayers Prepared by Sputtering”, Jpn. J. Appl. Phys. Vol. 41 , Part 1, No. 11B, pp. 6857–6861 (2002)
[2] W. T. Lim, K. R. Cho, C. H. Lee, “Structural and Electrical Properties of RF-sputtered RuO2 films having different conditions of preparation”, Thin Solid Films, Vol. 348, pp. 56-62 (1999)
[3] Y. Kaga, Y. Abe, H. Yanagisawa, K. Sasaki, “Formation Process and Electrical Property of RuO2 Thin Films Prepared by Reactive Sputtering”, Jpn. J. Appl. Phys. Vol. 37, Part 1, No. 6A , pp. 3457-3461 (1998)
[4] J. G. Lee, Y. T. Kim, and S. K Min and S. H. Choh, “Effects of excess oxygen on the properties of reactively sputtered RuOx thin films”, J. Appl. Phys. Vol. 77, No. 10, pp.5473-5475 (1995)
[5] S. Bhaskar, P. S. Dobal, S. B. Majumder, and R. S. Katiyar, “X-Ray Photoelectron Spectroscopy and Micro-Raman Analysis of Conductive RuO2 thin Films”, J. Appl. Phys., Vol. 89, No. 5, pp. 2987-2992 (2001)
[6] J. F. Moulder et al., “Handbook of X-Ray Photoelectron Spectroscopy”, Perkin-Elmer Corporation (1992)
[7] T. Maeder, P. Muralt, and L. Sagalowicz, “Growth of (111)-oriented PZT on RuO2 (100) / Pt (111) electrodes by in-situ sputtering”, Thin Solid Films, Vol. 345, pp. 300-306 (1999)

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