Solid-state NMR studies of the crystalline and amorphous domains within PEO and PEO: LiTf systems.

Solid-state NMR studies of the crystalline and amorphous domains within PEO and PEO: LiTf systems. Research Abstract Details 

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Solid-state NMR studies of the crystalline and amorphous domains within PEO and PEO: LiTf systems. Abstract Text:

Jason R Wickham,Rachel N Mason,Charles V Rice,

Solid polymer electrolytes (SPEs) contain amorphous and crystalline regions, each of which have unique contributions to the (13)C NMR spectrum. Understanding and assigning the (13)C NMR signals are vital to interpreting the NMR data collected for each phase. The (13)C CPMAS solid-state NMR spectrum of poly(ethylene oxide), a common polymer electrolyte host material, has superimposed broad and narrow components. Previously, the narrow component has been assigned to the amorphous region and the broad component to the crystalline PEO fraction. These assignments for pure PEO have been applied to various PEO:salt systems. Using lithium triflate salt dissolved in PEO, we revisit the spectral assignments and discover that the narrow component is due to crystalline PEO:LiTf component, which is reversed from the previous pure PEO assignment. This paradigm shift is based on data collected from a 100% crystalline PEO:LiTf with a 3:1 oxygen:lithium ratio sample, which exhibited only the narrow peak. For dilute electrolytes, such as 20:1 PEO:LiTf, the (13)C CPMAS spectra contain the narrow peak superimposed on a broad peak as seen with pure PEO. As dilute electrolytes are heterogeneous with crystalline and amorphous regions of both pure PEO and PEO:LiTf complex, peak assignments for pure PEO and PEO:LiTf are important. Thus, we reexamine the previous assignment for pure PEO using samples of pure powdered PEO, thermally treated pure powdered PEO, and a thin film PEO cast from an acetonitrile solution. With these different samples, we observed the growth of the narrow peak under conditions that favor crystallization. Therefore, for pure PEO, we have reassigned the narrow peak to the crystalline region and the broad peak to the amorphous region. In light of our observations, previous NMR studies of pure PEO and PEO SPEs should be reinvestigated. We also use rotational echo double resonance (REDOR) to study the 20:1 PEO:LiTf created from 2 and 100 kDa PEO. We find that the lithium environment is similar in the respective microcrystalline domains. However, the 100 kDa samples have a larger fraction of pure crystalline PEO.

Solid-state NMR studies of the crystalline and amorphous domains within PEO and PEO: LiTf systems. Publishing Authors By Initials

JR Wickham,RN Mason,CV Rice,

For similar inorganic chemicals: salts research abstracts see: inorganic chemicals: salts research

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Solid-state NMR studies of the crystalline and amorphous domains within PEO and PEO: LiTf systems. Journal Published:

PUBLICATION TYPE: Research Support, U.S. Gov't,

Journal: Solid state nuclear magnetic resonance

VOLUME: 31

Page Numbers: 184-92

Journal Abbreviation:

ISSN: 0926-2040

DAY: 13

MONTH: 05

YEAR: 2007

Solid-state NMR studies of the crystalline and amorphous domains within PEO and PEO: LiTf systems. Information

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LANGUAGE: eng

NlmUniqueID: 9306181

Solid-state NMR studies of the crystalline and amorphous domains within PEO and PEO: LiTf systems. Keywords Mesh Terms:

KEYWORDS: Salts

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Chemical & Substance for Abstract: Solid-state NMR studies of the crystalline and amorphous domains within PEO and PEO: LiTf systems. Information

Substance Name: Lithium

Registry Number: 7439-93-2

Grant and Affiliation Information for Solid-state NMR studies of the crystalline and amorphous domains within PEO and PEO: LiTf systems.

AFFILIATION: Department of Chemistry and Biochemistry, University of Oklahoma, 620 Parrington Oval, Room 208, Norman, OK 73019, USA.

Country: Netherlands

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MEDLINETA: Solid State Nucl Magn Reson

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