Characterization of Multi-Component Polymer Systems by Field Emission-STEM at Low Accelerating Voltages.

Shiraga, Noboru; Tanaka, Kozo; Minobe, Masao

doi:10.1295/koron.49.353

Cited by 4 publications

(3 citation statements)

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“…[21][22][23] Shiraga et al investigated the bulk phaseseparated structure of the immiscible PS/poly(methyl methacrylate) (PS/PMMA) blend film on the basis of field-emission scanning electron microscopic observation. 21 They revealed that macroscopic phase-separated domains with a few micrometers in diameter were formed in the bulk region of the thick film. Winnik and co-workers investigated the depth profiling of the phaseseparated structure for the PS/PMMA blend film on the basis of laser confocal fluorescence microscopic observation.…”

Section: Introductionmentioning

confidence: 99%

“…Internal phase-separated morphology for immiscible polymer blend films has been studied by several groups. − Shiraga et al investigated the bulk phase-separated structure of the immiscible PS/poly(methyl methacrylate) (PS/PMMA) blend film on the basis of field-emission scanning electron microscopic observation . They revealed that macroscopic phase-separated domains with a few micrometers in diameter were formed in the bulk region of the thick film.…”

Section: Introductionmentioning

confidence: 99%

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Film Thickness Dependence of the Surface Structure of Immiscible Polystyrene/Poly(methyl methacrylate) Blends

1996

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The film thickness dependence of surface structure for immiscible polystyrene/poly(methyl methacrylate) (PS/PMMA) films was investigated on the basis of atomic force microscopic observation and X-ray photoelectron spectroscopic measurement. In the case of the PS/PMMA film of 25 μm thickness, the air−polymer interfacial region was covered with a PS rich overlayer due to its lower surface free energy compared with that of PMMA and a well-defined macroscopic phase-separated structure was formed in the bulk phase. Also, in the case of the PS/PMMA thin film of 100 nm thickness, the phase-separated structure, in which the PMMA rich domains separated out of the PS rich matrix, formed at the film surface. The formation of the surface structure for the PS/PMMA thin film can be attributed to either the chain conformation or chain aggregation structure being frozen at the air−polymer interfacial region before the formation of a PS rich overlayer due to the fairly fast evaporation of solvent molecules. On the other hand, the two-dimensional PS/PMMA ultrathin film of 10.2 nm thickness did not show distinct phase-separated structure. When the film thickness became thinner than 10.2 nm, the two-dimensional PS/PMMA ultrathin film of 6.7 nm thickness showed fine and distinct phase-separated structure with the domain size of a few hundred nanometers. This structure can be designated as “mesoscopic phase-separated structure”. The surface phase state for the two-dimensional PS/PMMA ultrathin films can be explained by the film thickness dependence of both the interaction parameter and the degree of entanglement among polymer chains.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Film Thickness Dependence of the Surface Structure of Immiscible Polystyrene/Poly(methyl methacrylate) Blends

1996

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“…Cantow et al firstly attempted the imaging of distributions of low atomic number elements in some multiphase polymer materials with ESI mode in EFTEM_ 5 -7 However, no works have been appeared regarding the elemental distribution imaging for the polymers which have been frequently used as components for polymer alloys and blends such as polyamide (PA) and poly(methylmethacrylate) (PMMA). The reason for that may be the low sensitivity of N and O in EELS in specimens where carbon is the predominant element, 8 the loss of light elements through the radiation damage 9 and the difficulties for the preparation of thin unstained specimens especially for PA to be necessary for the reduction of the plural inelastic scattering. 10 Preparing thin unstained specimens less than 50 nm and introducing a "Imaging Plate" (IP) system for a recording medium, we here present the imaging of morphologies by elemental mapping in the blends ofpolyamide6 (PA6)/polycarbonate (PC) and polystyrene (PS)/PMMA.…”

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Energy-Filtering Transmission Electron Microscopy for the Characterization of Polymer Blend Morphologies

Horiuchi

Yase

Kitano

et al. 1997

Polym J

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KEY WORDSEnergy-Filtering Transmission Electron Microscopy (EFTEM) / Electron Energy Loss Spectroscopy (EELS) / Electron Spectroscopic Imaging (ES!) / Polymer Blend / Morphology / Much attention has been recently focused on energyfiltering transmission electron microscopy (EFTEM) as an analytical microscopy having a spatial resolution of less than a nanometer. 1 - 3 The EFTEM allows us to analyze element compositions by electron energy loss spectroscopy (EELS) and allows us to create an image by electron spectroscopic imaging (ESI) mode. The EELS gives us information on both qualitative and quantitative elemental compositions at local area of materials from the edge profiles of element specific ionization of inner shells. The ESI is an imaging technique which creates images with the unscattered electrons or the inelastically scattered electrons at selective energy losses. The "contrast tuning" and the "element specific contrast" obtained by ESI are a part of the useful features of ESl. 4 There are several works regarding the application of EFTEM to the morphological studies of multiphase polymer materials. Cantow et al. firstly attempted the imaging of distributions of low atomic number elements in some multiphase polymer materials with ESI mode in EFTEM_ 5 -7 However, no works have been appeared regarding the elemental distribution imaging for the polymers which have been frequently used as components for polymer alloys and blends such as polyamide (PA) and poly(methylmethacrylate) (PMMA). The reason for that may be the low sensitivity of N and O in EELS in specimens where carbon is the predominant element, 8 the loss of light elements through the radiation damage 9 and the difficulties for the preparation of thin unstained specimens especially for PA to be necessary for the reduction of the plural inelastic scattering. 10 Preparing thin unstained specimens less than 50 nm and introducing a "Imaging Plate" (IP) system for a recording medium, we here present the imaging of morphologies by elemental mapping in the blends ofpolyamide6 (PA6)/polycarbonate (PC) and polystyrene (PS)/PMMA. The IP has been recently developed as a recording medium for TEM. This system enables us to record a image at room temperature with very little irradiation damage by reducing electron dose to a specimen. 11 Moreover, we evaluate the quantitative aspects of EELS using the IP system. The IP allows us to record a electron energy loss spec-1 To whom correspondence should be addressed. 380 trum (EEL-spectrum) with wide range of energy losses more than 100 eV, with faster acquisition time less than one second and with wide dynamic range covering the electron dose from 2x 10-14 to 2x 10-9 Ccm-2 . 12 Hence physical drift and radiation damage of specimens which have been always occurred in EELS recording can be minimized. EXPERIMENT ALThe samples used in this study are the blends of polyamide6 and polycarbonate (PA6/PC) and polystyrene/ poly(methylmethacrylate) (PS/PMMA). The blends of PA6/PC (75/25 in weight ratio) and PS/PMMA (85/15) were ...

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Jar

Kuboki

Takahashi

1997

Journal of Materials Science Letters

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Characterization of Multi-Component Polymer Systems by Field Emission-STEM at Low Accelerating Voltages.

Cited by 4 publications

References 0 publications

Film Thickness Dependence of the Surface Structure of Immiscible Polystyrene/Poly(methyl methacrylate) Blends

Film Thickness Dependence of the Surface Structure of Immiscible Polystyrene/Poly(methyl methacrylate) Blends

Energy-Filtering Transmission Electron Microscopy for the Characterization of Polymer Blend Morphologies

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