Crystal structures, polymers amorphous phase

Classical X-ray diffraction and scattering is carried out in the subarea of wide-angle X-ray scattering (WAXS). The corresponding scattering patterns yield information on the arrangement of polymer-chain segments (e.g., orientation of the amorphous phase, crystalline structure, size of crystals, crystal distortions, WAXS crystallinity). 

As discussed above, many polymers contain some crystalline structures when they are solidified. These polymers are referred to as semicrystalline resins. These crystalline structures can be observed using microscopy as shown in Fig. 2.12 for PP and sPS resins. As shown schematically in Fig. 2.13 and discussed above, not all portions of the polymer chains are incorporated into the crystalline structure. Instead, the portions of the chains that are not crystallized make up the amorphous phase. Solid density is the most commonly used method for measuring the... 

Some polymorphic modifications can be converted from one to another by a change in temperature. Phase transitions can be also induced by an external stress field. Phase transitions under tensile stress can be observed in natural rubber when it orients and crystallizes under tension and reverts to its original amorphous state by relaxation (Mandelkem, 1964). Stress-induced transitions are also observed in some crystalline polymers, e.g. PBT (Jakeways etal., 1975 Yokouchi etal., 1976) and its block copolymers with polyftetramethylene oxide) (PTMO) (Tashiro et al, 1986), PEO (Takahashi et al., 1973 Tashiro Tadokoro, 1978), polyoxacyclobutane (Takahashi et al., 1980), PA6 (Miyasaka Ishikawa, 1968), PVF2 (Lando et al, 1966 Hasegawa et al, 1972), polypivalolactone (Prud homme Marchessault, 1974), keratin (Astbury Woods, 1933 Hearle et al, 1971), and others. These stress-induced phase transitions are either reversible, i.e. the crystal structure reverts to the original structure on relaxation, or irreversible, i.e. the newly formed structure does not revert after relaxation. Examples of the former include PBT, PEO and keratin. 

Dehydrated calcium pimelate is added (between 0.01 and 0.5 wt %) as the nucleating agent to isotactic polypropylene to produce the (3 modification of iPP [63]. Following molding between two glass plates at 220°C thin films of the polymer are isothermally crystallized at 140°C-143°C in a microscopy hot stage. After the hedritic structures develop, the samples are quenched to room temperature. Prior to AFM examination, the specimens are etched with a 1% solution of potassium permanganate in a mixture of sulfuric and orthophosphoric acid [64, 65]. This procedure is described in detail in the literature Caution consult the literature for safety precautions ) and helps to remove preferentially amorphous phase of PP [64]. Thus, unlike in the many other examples discussed in Sect. 3.2, here the interior of a specimen is analyzed after its exposure. 

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