漢朝古文物、南丹鐵隕石及微膠囊的特性與表面分析之研究

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研究生：	殷裕勝 Yin, Yu-Sheng
論文名稱：	漢朝古文物、南丹鐵隕石及微膠囊的特性與表面分析之研究 Characterization and Surface Analysis of the Antiques from Han Dynasty, Nan-Dan Iron Meteorite, and Microcapsules
指導教授：	凌永健 Ling, Yong-Chien
口試委員:
學位類別：	博士 Doctor
系所名稱：	理學院 - 化學系 Department of Chemistry
論文出版年：	2010
畢業學年度：	98
語文別：	英文
論文頁數：	137
中文關鍵詞：	青銅器、二次離子質譜儀、鐵隕石、微膠囊
外文關鍵詞：	Bronze, SIMS, Iron Meteorites, Microcapsule
相關次數：	點閱：2 下載：0
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Surface analysis with the capability of trace analysis and micro-area analysis has played an important role in scientific research. However, a diverse range of problems is difficult to dissolve by specific characterized techniques. Developing a suitable strategy containing of various analytical methods to study specific topic is useful in many fields. In this thesis, the ancient antiques from Han Dynasty (漢朝), Nan-Dan (南丹) iron meteorite, and polyelectrolyte microcapsules are investigated by modern analytical techniques, especially ToF-SIMS.
Han Dynasty is one of the most splendid times in Chinese culture. The manufacturing technology to art antiques in Han Dynasty is excellent in ancient China. Characterization of the objects though modern analytical techniques, such as XRF, ICP-MS and ToF-SIMS, is helpful to reveal the ancient wisdom and confirm the authenticity. The object was divided to two portions: (1) the lion consists of Cu/Zn alloy with a 20-30 贡m Ni layer for anticorrosion purpose; (2) the seal consists of a Pb base with a 225 贡m Cu layer and a 25汹贡m Ni layer on the topmost surface. Combination of ToF-SIMS and ICP-MS proved the gold exists on the lion surface and possibly deposited by ancient Chinese Liujin method. An identifying protocol for ancient antiques was established in this study for archaeology to discover the ancient technique and supply further information.
Nan-Dan iron meteorites, well known iron meteorites in the world, have been studied by various methods to identify the property, structure and composition. However, discovering the distribution of specific composition is difficulty due to the small size, wide concentration range, and unknown composition. In this study, the meteorite is investigated by SEM, ESCA and ToF-SIMS to acquire the morphology, chemical state and chemical ion images. Iron is distinguished to exist in three main types and the complex of iron binding with C, Si and Cl. Some nubbles with Cr shell were discovered by ion images. Both aggregations with Cu and Al/Si dominant textures display in the core area of these nubbles. This work contributes some fresh knowledge on Nan-Dan iron meteorites and demonstrates new application of ToF-SIMS.
Engineered polyelectrolyte multilayer (PEM) films of polyallylamine hydrochloride (PAH) and polystyrene sulfonate (PSS) assembled on polyethylene terephthalate (PET) substrate as well as PEM microcapsules of PAH and PSS templated onto polystyrene latex were fabricated by layer-by-layer assembly and characterized by various analytical techniques. The characteristic ion intensities from the respective outermost layer obtained by ToF-SIMS accorded well with the layer composition. The S and C8H7SO3 ion intensities were higher in PSS layers; whereas Cl ion intensity was higher in PAH layers. The SEM image displayed morphology which involved electrostatic interactions during the formation of multilayer. AFM measurement showed the shell thickness of PEM microcapsules as 1.21 nm. ToF-SIMS total ion, S ion, and Cl ion images were useful to delineate the PEM microcapsules location and to indicate successful assembly. The results demonstrated for the first time the feasibility of label-free ToF-SIMS imaging of PEM microcapsules.

Table of Contents
   Pages
List of Contents    I
List of Tables    IV
List of Figures    V
Chapter 1 Introduction
1-1  Surface Analysis Techniques    1-1
1-2  ToF-SIMS    1-3
     1-2-1  Basic principles    1-3
     1-2-2  Ion source and electron pulse    1-4
     1-2-3  Mass analyzer and detector    1-6
     1-2-4  Resolution    1-7
     1-2-5  Operation modes    1-8
     1-2-6  Data interpretation    1-10
     1-2-7  Applications    1-12
1-3  Motives    1-14
1-4  References    1-16
1.5  Tables    1-21
1.6  Figures    1-24
Chapter 2 Antiques from Han Dynasty Studied by Surface Analytical Techniques
2-1  Introduction    2-1
     2-1-1  Surface analytical techniques in archeology    2-1
     2-1-2  Dating    2-3
     2-1-3  Artifact    2-4
     2-1-4  Manufacturing techniques    2-5
2-2  Experimental section    2-6
     2-2-1  Sample    2-6
     2-2-2  Characterization    2-6



2-3  Results and discussion of lion    2-8
2-4  Results and discussion of official seal    2-10
2-5  Summary    2-12
2-6  Conclusions    2-13
2-7  References    2-15
2.8  Tables    2-20
2.9  Figures    2-27
Chap 3 Characterization of Nan-Dan Iron Meteorite through Surface Analytical Techniques
3-1  Introduction    3-1
     3-1-1  Surface analysis in cosmochemistry     3-1
     3-1-2  Meteorites    3-2
     3-1-3  Nan-Dan iron meteorites    3-3
3-2  Experimental section    3-4
     3-2-1  Sample    3-4
     3-2-2  Characterization    3-4
3-3  Results and discussion    3-6
     3-3-1  ICP-MS    3-6
     3-3-2  OM and SEM    3-6
     3-3-3  ESCA     3-6
     3-3-4  ToF-SIMS (Surface spectrum)    3-7
     3-3-5  ToF-SIMS (Ion image)    3-7
     3-3-6  ToF-SIMS (Ion image with pre-sputtering)    3-8
3-4  Conclusions    3-9
3-5  References    3-10
3.6  Tables    3-12
3.7  Figures    3-16



Chap 4 Layer-by-Layer Engineered Polyelectrolyte Microcapsules Studied by ToF-SIMS and Related Analytical Techniques
4-1  Introduction    4-1
     4-1-1  Microcapsules    4-1
     4-1-2  Preparation and characterization    4-1
     4-1-3  Applications    4-2
4-2  Experimental section    4-3
     4-2-1  Materials    4-3
     4-2-2  Fabrication    4-3
     4-2-3  Characterization    4-5
4-3  Results and discussion    4-6
     4-3-1  Evaluation of preparing solution    4-6
     4-3-2  Characterization of PEM films    4-7
     4-3-3  Characterization of microspheres    4-8
     4-3-4  Characterization of microcapsules    4-9
4-4  Conclusions    4-11
4-5  References    4-12
4.6  Tables    4-15
4.7  Figures    4-16
Chap 5 Summary and Prospective

List of Tables
   Pages
Table 1-1    The relationship between the depth regimes and applications    1-21
Table 1-2    Summary of the surface analysis techniques divided by the incident and emitted beam    1-22
Table 1-3    Ion source    1-23
Table 1-4    Comparison of different mass analyzers    1-23
Table 2-1    Absolute dating techniques    2-20
Table 2-2    The main constituent elements screened by XRF    2-21
Table 2-3    The main constituent elements determined by ICP-MS    2-22
Table 2-4    Results of ToF-SIMS depth profiles of Lion    2-23
Table 2-5    The ion intensity of seal cross sections in the specific area    2-24
Table 2-6    Comparison of Sn and Ni2    2-25
Table 2-7    Lead isotope ratio of seal    2-26
Table 3-1    The main constituent elements determined by ICP-MS    3-12
Table 3-2    The percentage of major element analyzed by ESCA    3-13
Table 3-3    Major element analyzed by ToF-SIMS spectrum    3-14
Table 3-4    Natural and experimental isotope ratio of specific elements    3-15
Table 4-1    The basic property of PAH and PSS solution by means of Zeta potential analyzer    4-15



List of Figures
   Pages
Fig. 1-1    The operation process of ToF-SIMS    1-24
Fig. 1-2    Diagram of the sputtering process for metal oxides.    1-25
Fig. 1-3    Dual beam sputter ion source    1-26
Fig. 1-4    Time diagram of dual beam system    1-27
Fig. 1-5    Pulsed low-energy electron source    1-27
Fig. 1-6    Schematics of ToF analyzer and detector    1-28
Fig. 1-7    Mass analyzer    1-29
Fig. 1-8    The schematic diagram of operation modes    1-30
Fig. 1-9    Schematic illustration of the PCA results    1-31
Fig. 2-1    Chronological spans of the major absolute dating methods    2-27
Fig. 2-2    The appearance of these artefacts    2-28
Fig. 2-3    ToF-SIMS positive ion depth profiles    2-29
Fig. 2-4    Distribution of elements in the cross-section of Lion    2-30
Fig. 2-5    Line scan of Ni and Cu    2-31
Fig. 2-6    Results of OM and surface spectrum    2-32
Fig. 2-7    Depth profiles of seal (S) surface    2-33
Fig. 2-8    3D Distribution of elements reconstructed from Figure 2.7    2-34
Fig. 2-9    Depth profile of seal (S) insdes    2-35
Fig. 2-10    Depth profiles of seal (S) determined by D-SIMS    2-36
Fig. 2-11    Distribution of elements in the cross-section of seal    2-37
Fig. 2-12    Line scan of Ni, Cu, and Pb in C-S    2-38
Fig. 2-13    Surface spectrum in cross-section of S-C    2-39
Fig. 2-14    Manufacturing process    2-41
Fig. 2-15    Surface spectrum of seal surface    2-42
Fig. 2-16    Distribution of lead isotopes in depth of seal (S) inside    2-43






Fig. 3-1    Nan-Dan iron meteorite    3-16
Fig. 3-2    Optical Microscopy    3-17
Fig. 3-3    SEM    3-17
Fig. 3-4    ESCA-survey scan    3-18
Fig. 3-5    ESCA-chemical state of specific element    3-18
Fig. 3-6    ToF-SIMS spectrum    3-22
Fig. 3-7    Ion image of Nan-Dan (Spot 3) in high mass resolution mode    3-23
Fig. 3-8    Ion image of Nan-Dan (Spot 3) in high image resolution mode    3-24
Fig. 3-9    Ion image of Nan-Dan (Spot 4) before sputtering    3-25
Fig. 3-10    Ion image of Nan-Dan (Spot 4) after sputtering    3-26
Fig. 4-1    Diagram of LbL    4-16
Fig. 4-2    Fabrication process    4-17
Fig. 4-3    SEM of PEM films    4-18
Fig. 4-4    Normalized peak intensity representing characteristic ions from the outermost layer of 4-layer PEM film    4-19
Fig. 4-5    Zeta potential of respective outermost shell    4-20
Fig. 4-6    SEM image of 10-shell PS/(PAH/PSS)5 microspheres    4-21
Fig. 4-7    SEM of microcapsules though different removing agent    4-22
Fig. 4-8    SEM images of 10-shell PS/(PAH/PSS)5 microcapsules    4-22
Fig. 4-9    AFM image of 10-shell PS/(PAH/PSS)5 microcapsules    4-23
Fig. 4-10    ToF-SIMS ion images of ~6-贡m 10-shell PS/(PAH/PSS)5 microcapsules    4-23

                                

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