The molecular structure of poly(biphenyl dianhydride-p-phenylenediamine) polyimide thin films by infrared spectroscopy: Thickness dependence of structure in the nano- to micrometer range

Journal of Polymer Science, Part B: Polymer Physics

Volumn 36, Issue 7, 1998, Pages 1247-1260

  Hietpas, Geoffrey D ^a   Allara, David L ^a  

^a PENNSYLVANIA STATE UNIVERSITY   (United States)

Author keywords

Infrared spectroscopy; Molecular structure; Polyimides; Thin films

Indexed keywords

ELLIPSOMETRY; INFRARED SPECTROSCOPY; MOLECULAR STRUCTURE; PLASTIC FILMS; SILICON; ULTRATHIN FILMS;

THICKNESS DEPENDENCE;

POLYIMIDES;

EID: 0032069496     PISSN: 08876266     EISSN: None     Source Type: Journal    
DOI: 10.1002/(SICI)1099-0488(199805)36:7<1247::AID-POLB14>3.0.CO;2-8     Document Type: Article

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46. iso = 1.80, the value used in Figure 3.
47. 2 layer thicknesses, ∼ 2 nm, determined from ellipsometry. Interference fringe corrections were applied [see next footnote, ref. 30]. In constructing the orientational character of the polyimide film tensor it was assumed that the polymer chains and the ring planes were oriented parallel to the substrate, in line with the generally held structure of the thin films (see text).
48. Interference fringes can arise in simulated transmission spectra of parallel-layer film structures, due to the perfect parallel character and infinite sharpness of the interfaces. The interference intensity oscillations often can be huge, and failure to account for them can give rise to serious errors. Experimentally, the fringes are typically removed by the use of imperfect samples with slightly off-parallel faces and nonuniform interfaces. In the case of our Si supported transmission samples, the fringing is minimized by using wafers that are wedged across the face at an angle of ∼ 0.25-0.5°, thus effectively cancelling oscillation intensities because of the random phases. Analogously, for each simulation, we typically carry out ∼ 50-100 runs over a spread of small Si thicknesses and average them.
49. g during imidization, which constrains annealing. These density differences are of the appropriate magnitude to explain the observed discrepancies between simulation and experiment discussed above.
50. -1 for all film thicknesses, indicating a similar environment in the PDA phenyl ring for all of the thin films.
51. 2/air multilayered structure and consequently cannot be used for accurate estimation of film thicknesses for other types of BPDA-PDA films, e.g., free-standing films.
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53. 19 However, for normal incidence transmission spectra, simulations show that the observed asymmetry is much too strong to be accounted for by a single oscillator, regardless of its position and linewidth.
54. However, for extremely thin films of 2-5 nm thicknesses we experimentally observe a variation of imide ring structures such that while the vast majority of films possessed the highest densities of planar, stacked rings, a few had a larger fraction of perturbed imide rings, similar to the 100 nm films, indicating a greater sensitivity to imidization conditions for samples < 50 Å.
55. as(C=O) band asymmetry.
56. as(C=O) in-plane mode, which could be used as evidence for unperturbed imide rings.
57. PDA band intensities indicate that the polymer chains are aligned parallel to the substrate surface, domain rotation is restricted to around the chain axes, an unlikely physical situation.
58. These data indicate the presence of a complex ensemble of different imide ring configurations along the aligned chain axes with three types of imide ring configurations only at a lower limit. These populations are dynamic because, upon release of the stress at room temperature, it was observed that the Imide I and II line shapes gradually return to the unstretched values over several hours. Details will be reported elsewhere (see ref. 16).
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