Recent Advances in Transmission Electron Microtomography for Polymer Research

Jinnai, Hiroshi; Morita, Hiroshi; Niihara, Ken Ichi

doi:10.1295/koron.65.547

Cited by 5 publications

(1 citation statement)

References 81 publications

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“…Preparation of the ca. 100-nm thick cross-section samples of these nanocomposites by FIB milling requires optimization of ion beam parameters and of masking layers to avoid damaging the sensitive PEM modules. , A layer of evaporated carbon (ca. 20–200 nm) does not significantly perturb the underlying nanocomposite and provides protection during FIB milling.…”

Section: Resultsmentioning

confidence: 99%

Layer-by-Layer Assembly of Heterogeneous Modular Nanocomposites

et al. 2012

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Materials and MethodsGold nanoparticles. The gold colloid dispersion was prepared as previously described in the literature (ref 17). Briefly, a 100 mL of stock Au(III) aqueous solution was prepared from 1.00 g tetrachloroauric acid (HAuCl 4 , ≥99.9% purity, Aldrich) in an amber volumetric flask. The stock solution then was aged for one month in the dark.Before preparing the Au colloid, an Ehrlenmeyer flask and a Teflon® stirbar were cleaned by soaking in aqua regia (3:1 mixture of HCl and HNO 3 ) for 20-30 min, followed by a triple rinse in deionized water, and drying overnight in an oven at 110°C. Caution: Aqua regia solutions are extremely corrosive and may result in explosion or skin burns if not handled properly. A mixture of 1 mL of the stock Au(III) solution and 100 mL of deionized water was added to the clean flask, the flask then was covered loosely with a watch glass and the stirred contents were brought to a gentle boil. A 2.5 mL aliquot of an aqueous solution containing 1% wt. trisodium citrate (99%, Aldrich) was quickly added to the stirred contents of the flask. After formation of a clear, cherry red sol, it was gently boiled for an additional 10 min to complete the reduction, then allowed to cool to room temperature covered with the watch glass. The stirbar was removed, deionized water was added to return the volume to 100 mL, and the flask was capped tightly and stored for later use.Substrate cleaning. Two types of substrates were used for LbL assembly: polished fused silica slides (Dell Optics, Inc.) and single-side-polished Si wafers (n-type, As-doped, <100> orientation, Recticon Corp.) For initial cleaning, Si wafers and fused silica slides were placed in a slotted Coplin jar and covered with a 1:1 v/v mixture of methanol and concentrated HCl. The jar was loosely capped and allowed to stand for 45 min in a fume hood. Then the cleaning solution was drained and the substrates were thoroughly rinsed with deionized water. After draining the water, the substrates were covered with concentrated H 2 SO 4 and allowed to stand for 45 min in the loosely capped jar. The sulfuric acid then was decanted away and the substrates were thoroughly rinsed with deionized water.Substrate modification. After cleaning, the substrates were modified by chemisorption of EDA (N-(2-aminoethyl)-N-3aminopropyltrimethoxysilane, Gelest, Inc.) The EDA solution was prepared by adding 2 mL of EDA to 200 mL of deionized water, mixing to dissolve the EDA, and then adding 240 µL of glacial acetic acid. The clean substrates were covered with the EDA solution for 30 min at room temperature then thoroughly rinsed with deionized water. Immediately after the final rinse, the substrates were dried in a filtered N 2 gas stream, baked 6-8 min in an oven at 110-120°C, cooled, and stored in plastic containers.Polyelectrolyte solutions. A stock solution of 1.00 M NaCl (aq) was prepared in a volumetric flask by dissolving 58.

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Section: Resultsmentioning

confidence: 99%

Layer-by-Layer Assembly of Heterogeneous Modular Nanocomposites

et al. 2012

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New opportunities in transmission electron microscopy of polymers

Kuei

Aplan

Litofsky

et al. 2020

Materials Science and Engineering: R: Reports

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Recent Advances in Multi-Scale Tomographic Techniques in Polymer Research

Jinnai¹

2012

KOBUNSHI RONBUNSHU

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要旨近年，高分子の不均一構造を三次元的に実空間観察することにより高分子材料の評価・解析に資する一連の顕微鏡群が注目を浴びている．これらの中にはトモグラフィー (ギリシア語で slice を意味する "tomos" と image を意味する "graph" の造語) を基盤とするものが多い．本報では高分子材料分野でと

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Recent Advances in Transmission Electron Microtomography for Polymer Research

Cited by 5 publications

References 81 publications

Layer-by-Layer Assembly of Heterogeneous Modular Nanocomposites

Layer-by-Layer Assembly of Heterogeneous Modular Nanocomposites

New opportunities in transmission electron microscopy of polymers

Recent Advances in Multi-Scale Tomographic Techniques in Polymer Research

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