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Visualization of Macromolecules and Polymer Morphology

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Scanning Force Microscopy of Polymers

Part of the book series: Springer Laboratory ((SPLABORATORY))

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Abstract

Polymers and their morphology are characterized by a structural hierarchy on different levels, which belong to molecular, nanometer, mesoscopic, micrometer, and macroscopic length scales, respectively. The analysis of the underlying structure by means of scanning force microscopy (SFM) on the relevant length scale, and in particular the interpretation of SFM micrographs, requires some basic concepts of polymer morphology. This chapter reviews some rudimentary concepts of structural hierarchy in polymers and hence lays the ground for the hands-on SFM examples discussed in later chapters.

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Notes

  1. 1.

    For safety precautions see your suppliers manual and warnings.

  2. 2.

    This piezo transducer was damaged by accidental feed with high uncontrolled voltages, the resulting damage and its manifestation in AFM scans, however, is very similar.

  3. 3.

    In the case of a leakage the set up must be disassembled and carefully dried immediately to prevent damage of the scanner or the electronics.

  4. 4.

    A practical limitation for the approach in the field of polymers is the fact that shear forces, similar to contact mode, may cause sample damage or distortion of the underlying morphology.

  5. 5.

    Mica can be conveniently cleaved by placing a piece of pressure sensitive adhesive on top of a planar mica specimen. The tape is carefully peeled off the surface, thus exposing a near atomically smooth, clean surface. In ambient conditions this very hydrophilic surface is rapidly covered with airborne adsorbates.

  6. 6.

    The setpoint amplitude is adjusted to ∼0.9 A0 to 0.95 A0. If the tip loses track of the surface during scanning, the setpoint must be slightly reduced. Next the scan size is stepwise increased while the gains are optimized accordingly, which corresponds to vanishing contrast in the amplitude image.

  7. 7.

    The EPDM rubber used was Keltan® 512, produced by DSM Elastomers. Pure precipitated silica (Ultrasil® VN3) and silica modified with the organosilane (Si 69), as well as carbon black (N 550) were employed as fillers. Masterbatches without curing additives were mixed in a Shaw K1 Mark IV intermeshing mixer of DSM Elastomers Europe BV. Mixing was stopped once the compounds reached a temperature of ca. 110° C. The mixing conditions are given in below. Masterbatches without curing additives were mixed in a Shaw K1 Mark IV intermeshing mixer of DSM Elastomers Europe BV. Mixing was stopped once the compounds reached a temperature of ca. 110° C. The mixing conditions are given in further below.

    Ingredients (phr)

    1

    2

    Kelton® 512

    100

    100

    ZnO

    3

    3

    Stearic acid

    1

    1

    Ultrasil®VN3

    50

    –

    Si 69

    4

    –

    Sunpar® 2280

    30

    30

    MBT

    –

    –

    TMTD

    –

    –

    Sulfur

    –

    –

    N 550

    –

    50

    Mixer acquisition

    1

    2

    Load factor (%)

    54

    54

    Power max (kW)

    50

    49

    Power end (kW)

    40

    37

    Tbatch max (oC)

    113

    108

    Tbatch end (oC)

    112

    107

    E motor (MJ/m3)

    7

    6

    E water (MJ/m3)

    56

    −7

    Mix time (sec)

    312

    205

  8. 8.

    Caution! Consult appropriate literature and ensure that safety regulations are being followed. Strong oxidants and acids are used. Conditions: 0.7 % w/v of potassium permanganate in a mixture of sulfuric acid (95-97%, Merck) and phosphoric acid (85%, Aldrich) in the volumetric ratio of 2:1. Specimens are etched in 0.7 % w/v of the permanganic solution at room temperature typically over 5 h. The etched samples are washed with a diluted sulfuric acid in the volume ratio of 2:7 in distilled water, which is cooled to near the freezing point with ice to prevent the heat of dilution of the original acids from affecting the sample surface. This solution is subsequently decanted. The samples are then washed with hydrogen peroxide (35%) to reduce any remaining manganese dioxide or permanganate. The final step is to wash the sample(s) several times with distilled water, and finally with acetone.

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Authors and Affiliations

  1. Physikalische Chemie, Universität Siegen, Adolf-Reichwein-Str. 2, 57068, Siegen, Germany

    Prof. Dr. Holger Schönherr

  2. MESA+ Institute for Nanotechnology Materials Science and Technology of Polymers, University of Twente, 217, 7500, AE, Enschede, The Netherlands

    Prof. Dr. G. Julius Vancso

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  1. Prof. Dr. Holger Schönherr
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  2. Prof. Dr. G. Julius Vancso
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Correspondence to Holger Schönherr .

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Schönherr, H., Vancso, G.J. (2010). Visualization of Macromolecules and Polymer Morphology. In: Scanning Force Microscopy of Polymers. Springer Laboratory. Springer, Berlin, Heidelberg. https://doi.org/10.1007/978-3-642-01231-0_3

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