先端分析・評価技術
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1 Advanced Analytical and Evaluation Techniques LSI FE-TEM STEM 1 nm 2 Abstract The structure of devices such as next-generation LSIs and magnetic heads is becoming increasingly fine and complicated, making it necessary to control the thickness, composition, and fine structure of thin films for the devices at the nanometer level. Such control requires techniques for analyzing and evaluating thin films at the nanometer level. In this paper, we assess the present and future needs for analysis and evaluation techniques, suggest cutting-edge techniques that should be developed, and introduce the current status of our work on developing such techniques. First, we describe techniques for analyzing the structure and composition of fine structures at the nanometer level by using high-angle annular dark-field (HAADF) STEM, which enables each element to be identified, as well as field-emission (FE) type TEM. Next, we present details of low voltage secondary ion mass spectrometry (LV-SIMS) for analyzing the depth profile of trace quantities of impurities with a depth resolution of less than 1 nm. Finally, we introduce the current status of our development of electron holography, which permits visualization of both the electrical and magnetic properties as well as fine structure of materials with nanometer-level spatial resolution. 現在, ナノレベルの分析 評価技術の開発, ナノ成膜 制御技術の開発に従事 現在, 二次イオン質量分析法を用いた高精度微量不純物分析技術の開発に従事 382 FUJITSU.52, 4, p (07,2001)
2 LSI GMR CMOS HDD GMR -1 1 nm nm 次世代デバイス開発に不可欠なナノレベル分析 評価技術 5 ゲート絶縁膜の膜厚 (nm) MR GMR 年 ( 西暦 ) TMR CMR -1 Fig.1-Change of thicknesses of thin films in major parts of CMOS and GMR head. ヘッド用薄膜の最小膜厚 (nm) 1 Field Emission Type Transmission Electron Microscope FE-TEM TEM HR- TEM TEM STEM / X Energy Dispersive X-ray Spectroscopy EDX (1) High Angle Anular Dark-Field Scanning Transmission Electron Microscopy HAADF-STEM (2) 2 CMOS Electron Energy Loss Spectroscopy EELS (3) 1 FE-TEM 3 ppb Si-LSI SIMS Secondary Ion Mass Spectrometry p nnm B As P 2 2SIMS SIMS (4) Atomic Force Microscope AFM Scanning Capacitance Microscopy SCM (5) Si FUJITSU.52, 4, (07,2001) 383
3 nm 4 Scanning Probe Microscopy SPM (6) Scanning Maxwell Stress Microscopy SMM 2 FE-TEM 分析ニーズ ナノ ~ サブナノ領域の構造解析 組成分析 ナノ領域の状態 ( 結合, 化学状態 ) 評価 ナノ領域の微量 (ppb レベル ) 分析 ナノレベルの電気的現象の可視化 ナノレベルの磁気的現象の可視化 分析技術 FE-TEM/EDX HAADF-STEM STEM-EELS 微小領域 SIMS,SCM 極微量化学分析 走査フ ローフ 顕微鏡法 電子線ホロク ラフィー スピン STM -2 Fig.2-Nano-meter lebel analytical techniques essential for the development of next generation devices. 5 NiFe Co STM Scanning Tunneling Microscopy -2 HR-TEM HAADF-STEM HR-TEM HAADF-STEM (1) HR-TEM HR-TEM Si(Z=14) nm a Si 110 b ahr-tem c ahaadf-stem -3 Si 110 TEM a Si 110b ahr-temc ahaadf-stem Fig.3-High resolution TEM observation of Si(110) cross-section. (a) Atomic arrangement of Si crystal viewed from the (110) cross-section; (b) An HR-TEM image corresponding to (a) ; (c) An HAADF-STEM image corresponding to (a). 384 FUJITSU.52, 4, (07,2001)
4 110-3 a HR-TEM-3 b Si 入射電子線 0.2 nmφ TEM 試料 高角散乱電子 -4 HAADF-STEM Fig.4-Schematic diagram for a principle of HAADF-STEM. HAADF-STEM HAADF-STEM -4 annular detector Z Z 0.2 nmfe-tem -3 c -3 ahaadf-stem 2 Si-5 agaas 110 HAADF-STEM-5 b 33 As 31 Ga As AlAs/GaAs GMR NiFe/Co/Cu/Co HR-TEM Ga(Z=31) As(Z=33) nm a GaAs 110 b ahaadf-stem -5 GaAs 110 HAADF-STEM a GaAs 110b ahaadf-stem Fig.5-HAADF-STEM observation of GaAs(110) cross-section. (a) Atomic arrangement of GaAs crystal viewed from the (110) cross-section; (b) An HAADF-STEM image corresponding to (a). FUJITSU.52, 4, (07,2001) 385
5 SIMS 2SIMS CMOS 2.5 nm 40 nm B As 1 nm SIMS (7) 1 1 kev (8)-(10) 1 (11) 5.0 nm 1 Cs 0.5 kev2 質量分析 1 次イオンの照射 2 次イオンの検出 asem SIMS Fig.6-Schematic diagram for a priciple of secondary ion mass spectrometry (SIMS) 二次イオン強度 2 ( ( 任意単位 ) NCs bsem 深さ (nm) 図 -7 Fig.7-Depth profile of nitrogen atoms in a silicon oxinitride film. -8 Cs 1SEM a 1 75b 1 55 Fig.8-Scanning electron micrographs of surfaces of the samples after irradiation of Cs + primary ions. (a) Incident angle of primary ions: 75 degrees; (b) 55 degrees. 386 FUJITSU.52, 4, (07,2001)
6 NCs Cs 1 NCs NCs nm 1 kev 1 Cs 1-8 ab Scanning Electron Microscope SEM Cs m Ga SIMS Pb(Ti,Zr)O3(PZT) FRAM (12)-(14) TEM 電子銃 収束レンズ Bi-prism の役割 試料 対物レンズ 電子複プリズム (Bi-prism) ホログラム スクリーン ホログラム -9 Fig.9-Schematic diagram for a principle of off-axis electron holography. FUJITSU.52, 4, (07,2001) 387
7 (15) Arahanov- Bohm (16) (17) 20 (18) offaxis -9 (19) Field Emission Gun FEG 1 FEG 2 bi-prism bi-prism TEM 3 TEM 4 TEM nm a PZT TEM b a c b -10 a PZT TEMb ac b Fig.10-Evaluation of ferroelectric film by electron holography. (a) A cross sectional TEM image of the PZT film and the bottom electrode; (b) An electron hologram of correponding to (a); (c) A phase image correponding to (b). 388 FUJITSU.52, 4, (07,2001)
8 FRAM PZT / TEM-10 abc -10 a TEM-10 b-10 a -10 c -10 b -10 a -10 c PZT 1 J. J. Hren et al. Introduction to Analytical Electron Microscopy Prenum Press New York P. D. Nellist et al. Subangstrom Resolution by Underfocused Incoherent Transmission Electron Microscopy Phys. Rev. Lett. Vol.81 p R. F. Egerton Electron Energy-Loss Spectroscopy in the Electron Microscope, 2 nd ed. Plenum Press New York FIB SIMS Vol.21 p C. C. Williams et al. Lateral dopant profiling with 200 nm resolution by scanning capacitance microscopy Appl. Phys. Lett. Vol.55 p W. Shen et al. Investigation of the Radial Compression of Carbon Nanotubes with a Scanning Probe Microscope Phys. Rev. Lett. Vol.84 p K. Wittmaack et al. Sources of error in quantitative depth profiling of shallow doping distributions by secondary-ion-mass spectrometry in combination with oxygen flooding J. Vac. Sci. Technol. Vol.B16 p Z. X. Jiang et al. Secondary ion mass spectrometry and atomic force spectroscopy studies of surface roughning, erosion rate change and depth resolution in Si during 1 kev 60 O 2 bombardment with oxygen flooding J. Vac. Sci. Technol. Vol.B16 p K. Wittmaack Influence of the depth calibration procedure on the apparent shift of impurity depth profiles measured under conditions of long-term changes in erosion rate J. Vac. Sci. Technol. Vol.B18 p Y. Kataoka et al. Ion-induced electron emission as a means of studying energy- and angle-dependent compositional changes of solids bombarded with reactive ions II Nitrogen bombardment of silicon Surf. Sci. Vol.424 p Y. Kataoka et al. Characterization of ultra-thin oxynitrides by MCs SIMS Detailed evaluation of the dependence of ion yields and surface roughening on beam energy and impact angle Proc. of Int. Workshop on Fabrication, Characterization, and Modeling of Ultra- FUJITSU.52, 4, (07,2001) 389
9 Shallow Doping Profiles in Semiconductors p T. D. Hadnagy Materials and Production Characterization Requirements for the Production of FRAMR Memory Products Proceedings of the 9th International Symposium on Integrated Ferroelectrics p J. F. Roeder et al. MOCVD of Ferroelectric and Advanced Dielectric Thin Films by Liquid Delivery Proceedings of the 9th International Symposium on Integrated Ferroelectrics p T. J. Boyle et al. Non-Traditional Solution Routes to Ferroelectric Materials Proceedings of the 9th International Symposium on Integrated Ferro-electrics p A. Tonomura Application of Electron Holography Review of Modern Physics Vol.59 p July A. Tonomura Phys. Rev. Lett. Vol.54 p G. Matteucci Electron Holography of Long-Range Electric and Magnetic Fields J. Appl. Phys. Vol.69 p February J. M. Cowley Twenty forms of electron holography Ultramicroscopy Vol.41 p D. C. Joy Practical Aspect of Electron Holography Ultramicroscopy Vol.51 p FUJITSU.52, 4, (07,2001)
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