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10 Y. Yu, X. Wang / Extreme Mechanics Letters ( ) – Fig. 7. (a, b) Cross-sectional SEM images (i) and EDS mappings of a pristine PDMS film (a) and an AlOx-doped PDMS film (b) for Al, Si, O, and C elements (ii-v). (c) Full range XPS spectra acquired from pristine PDMS and AlOx-doped PDMS. Small Al 2p peak was identified on the spectrum of AlOx-doped PDMS. (d) Al 2p scan for pristine PDMS, AlOx-doped PDMS film and ALD grown Al2O3 on silicon substrate. The peak position shift indicates the presence of defective oxides in AlOx-doped PDMS film. (e) Dielectric constant measured from pristine PDMS and AlOx-doped PDMS, showing increased dielectric constant of PDMS due to the AlOx doping. Source: Reprinted with permission from Ref. [79]. © 2015, Wiley-VCH polished off for more than 2 μm. AlOx was selected as the dopants since trimethylaluminum (TMA, ALD precursor of Al2 O3 ) has desirable permittivity in a number of polymers such as polystyrene (PS), PP, polyethylene (PE), and poly(vinyl chloride) (PVC) and PMMA [73]. The SIS doping process was carried out in a homemade ALD system by sequentially introducing TMA and H2O vapor to the polymer film at 80 °C with controlled exposure time and cycles. Fig. 7(a) and (b) show the cross-sectional SEM images and corresponding energy dispersive spectroscopy (EDS) elemental mappings of the pristine PDMS film and the same film after 5-cycle sequential TMA/H2O infiltration (marked as AlOx -doped PDMS), respectively. PDMS elements including silicon (Si), oxygen (O) and carbon (C) were all identified with a uniform distribution in the pristine film and no aluminum (Al) signal was detected (Fig. 7(a-ii-v)). For the SIS-treated PDMS, Al signal was clearly detected and was concentrated within the top ∼3 μm region, revealing the effective infiltration depth (Fig. 7(b-ii)). Similarly, both O and C elements exhibited a concentrated signal within the top ∼3 μm region matching well with Al distribution (Fig. 7(b-iv) and (v)). The concentrated O element was originated from Al–O bonds formed after H2O molecule infiltrated into polymers and reacted with TMA. The unreacted methyl groups on TMA could be the main source responsible for the concentrated C signal. This elemental distribution analysis evidences the successful deep infiltration of both precursors in the polymer film and no surface coating of Al2 O3 was identified. XPS characterizations further confirmed the presence of Al element in the PDMS after the SIS infiltration. As shown in Fig. 7(c), a small peak of Al 2p appeared at the low binding energy region from the AlOx -doped PDMS film. The high resolution scan of Al 2p signal demonstrated a peak shift from 75.6 to 74.7 eV after the SIS treatment, which was caused by the formation of the defective aluminum oxides such as Al2O and AlO (Fig. 7(d)) [80]. The nonstoichiometric aluminum oxide may introduce extra charge carrier sites and thus improve the charge capacitance of the modified PDMS film. This hypothesis was verified by the dielectric constant measurement (Fig. 7(e)). SIS doping increased the dielectric constant of PDMS films from ∼2.4 to ∼2.7 within the test frequency range, implying that modified PDMS was capable of storing more charges compared with the pristine one.PDF Image | Chemical modification of polymer surfaces for advanced triboelectric nanogenerator development
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