Measurements of electron beam damage for organic crystals in a high voltage electron microscope with image plates

Ohno, Tamotsu; Sengoku, Masaya; Arii, Tatsuo

doi:10.1016/s0968-4328(01)00023-3

Cited by 13 publications

(3 citation statements)

References 16 publications

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“…2). We attribute this over-conversion to classical electron beam damage of polymers555657 which is a well-known problem in electron-microscopy. Due to the strong evidences that ideal doses convert TMSC into cellulose (OR), it logically follows, that for very low doses an incomplete conversion takes place.…”

Section: Resultsmentioning

confidence: 99%

Direct-Write Fabrication of Cellulose Nano-Structures via Focused Electron Beam Induced Nanosynthesis

Ganner

Sattelkow

Rumpf

et al. 2016

Sci Rep

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In many areas of science and technology, patterned films and surfaces play a key role in engineering and development of advanced materials. Here, we introduce a new generic technique for the fabrication of polysaccharide nano-structures via focused electron beam induced conversion (FEBIC). For the proof of principle, organosoluble trimethylsilyl-cellulose (TMSC) thin films have been deposited by spin coating on SiO2 / Si and exposed to a nano-sized electron beam. It turns out that in the exposed areas an electron induced desilylation reaction takes place converting soluble TMSC to rather insoluble cellulose. After removal of the unexposed TMSC areas, structured cellulose patterns remain on the surface with FWHM line widths down to 70 nm. Systematic FEBIC parameter sweeps reveal a generally electron dose dependent behavior with three working regimes: incomplete conversion, ideal doses and over exposure. Direct (FT-IR) and indirect chemical analyses (enzymatic degradation) confirmed the cellulosic character of ideally converted areas. These investigations are complemented by a theoretical model which suggests a two-step reaction process by means of TMSC → cellulose and cellulose → non-cellulose material conversion in excellent agreement with experimental data. The extracted, individual reaction rates allowed the derivation of design rules for FEBIC parameters towards highest conversion efficiencies and highest lateral resolution.

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Section: Resultsmentioning

confidence: 99%

Direct-Write Fabrication of Cellulose Nano-Structures via Focused Electron Beam Induced Nanosynthesis

Ganner

Sattelkow

Rumpf

et al. 2016

Sci Rep

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“…Here we have included an updated version of the graph showing the correlation between beam stability and thermal stability presented by Kumar and Adams (Fig. 5), showing additional studies from the literature23–33 and others published more recently 34–40…”

Section: Damage Sensitivitymentioning

confidence: 99%

High resolution electron microscopy of ordered polymers and organic molecular crystals: Recent developments and future possibilities

Martin

Chen

Yang

et al. 2005

J Polym Sci B Polym Phys

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High Resolution Electron Microscopy (HREM) has made it possible to directly image the detailed organization of a variety of polymers and organic molecular crystals. For organic materials it is imperative to use low dose techniques that minimize the structural reorganizations that inevitably occur during electron beam irradiation. This article reviews recent developments in low dose HREM from our own laboratory and elsewhere. The developments in closely related microstructural characterization techniques are also reviewed. In the future, the ability to correct the spherical aberration of the objective lens, the use of low voltages to increase contrast, and the use of time resolved techniques are expected to open new avenues for the ultrastructural investigations of organic materials. New sample preparation techniques, such as the ability to make thin samples by focused ion beam (FIBs), to cut samples with an oscillating diamond knife, and to more conveniently prepare cryogenically solidified specimens,are also expected to be of increasing importance

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“…The radiation damage to organic or inorganic materials occurs within the molecule, which can cause chemical bonds to break or to form crosslinks, and leads to molecule deformation and shifts from its original position. [1][2][3] In wet mode (lower vacuum), the radiation damage to a specimen not only results from the electron beam energy, but can also be exacerbated as a consequence of the water vapour present inside the chamber of ESEM. The water droplets can insulate and hydrate the specimen, while ionised water molecules can accelerate specimen degradation.…”

Section: Introductionmentioning

confidence: 99%

Investigation of radiation damage to microcapsules in environmental SEM

Ren¹,

Donald²,

Zhang³

2007

Materials Science and Technology

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The radiation damage to a specimen in the chamber of electron microscopes has been studied extensively in the past few years. However, for the specific case of specimens with a core/shell structure, such as microcapsules and biological cells, there has been little experimentation devoted to understanding how the radiation may affect their mechanical properties. In the present work, single melamine formaldehyde (MF) microcapsules were imaged using an environmental electron microscope (ESEM) under both dry and wet modes under conditions of different accelerating voltages. The changes in the morphology (shape) were monitored as a function of radiation time. In addition, a newly developed ESEM based nanomanipulation technique was used to measure how the force imposed on single MF microcapsules for a given deformation changed with radiation time, in order to identify a time window within which the radiation damage to the microcapsules may be negligible in order to be able to study the mechanical properties of the particles. Based on the findings, the nanomanipulation technique was applied to measure the force versus displacement for compressing single microcapsules to rupture, including determination of their rupture mode.

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Measurements of electron beam damage for organic crystals in a high voltage electron microscope with image plates

Cited by 13 publications

References 16 publications

Direct-Write Fabrication of Cellulose Nano-Structures via Focused Electron Beam Induced Nanosynthesis

Direct-Write Fabrication of Cellulose Nano-Structures via Focused Electron Beam Induced Nanosynthesis

High resolution electron microscopy of ordered polymers and organic molecular crystals: Recent developments and future possibilities

Investigation of radiation damage to microcapsules in environmental SEM

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