Preparation of organic-inorganic hybrids possessing nanosheets with perovskite-related structures via exfoliation during a sol-gel process

Seiichi Tahara, Yosuke Takeda, Yoshiyuki Sugahara

    Research output: Contribution to journalArticle

    39 Citations (Scopus)

    Abstract

    Organic-inorganic hybrids containing exfoliated nanosheets with a perovskite-related structure have been prepared from an n-decoxy derivative of an ion-exchangeable layered perovskite, HLaNb2O7· xH2O (HLaNb) or HCa2Nb3O10· xH2O (HCaNb), silanol-terminated poly(dimethylsiloxane) (PDMS), and tetramethoxysilane (TMOS) via a sol-gel process involving the reaction of the n-decoxy derivative with a PDMS-TMOS mixture and subsequent intentional hydrolysis with hydrochloric acid. The X-ray diffraction (XRD) patterns of the resultant products after intentional hydrolysis indicate both preservation of the perovskite-like slab structure and disappearance of stacking order. Partial exfoliation of layered perovskites is correspondingly observed by transmission electron microscopy (TEM). The formation of a polysiloxane network composed of PDMS chains and Qn units ((RO)4-nSi(OSi)n: R = H, CH3) via intentional hydrolysis is shown by the solid-state 29Si CP/MAS (cross-polarization and magic angle spinning) NMR spectroscopy. These products are expected to possess the Nb-O-Si linkage interface since a signal assignable to the (SiO)Si(CH3) 2O-Nb environment is present in the 29Si CP/MAS NMR spectra of products prepared from an n-decoxy derivative of HLaNb (or HCaNb), PDMS, and TMOS in a similar manner without intentional hydrolysis and the Nb-O-Si bonds are expected to be preserved during hydrolysis. The exfoliated structures should be formed during the intentional hydrolysis process since the products prepared without intentional hydrolysis clearly exhibit a stacking order along the c axis.

    Original languageEnglish
    Pages (from-to)6198-6204
    Number of pages7
    JournalChemistry of Materials
    Volume17
    Issue number24
    DOIs
    Publication statusPublished - 2005 Nov 29

    Fingerprint

    Nanosheets
    Perovskite
    Sol-gel process
    Hydrolysis
    Polydimethylsiloxane
    Magic angle spinning
    Derivatives
    Polarization
    Siloxanes
    Hydrochloric Acid
    Hydrochloric acid
    perovskite
    Silicones
    Diffraction patterns
    Nuclear magnetic resonance spectroscopy
    Nuclear magnetic resonance
    Ions
    Transmission electron microscopy
    X ray diffraction
    silanol

    ASJC Scopus subject areas

    • Materials Chemistry
    • Materials Science(all)

    Cite this

    Preparation of organic-inorganic hybrids possessing nanosheets with perovskite-related structures via exfoliation during a sol-gel process. / Tahara, Seiichi; Takeda, Yosuke; Sugahara, Yoshiyuki.

    In: Chemistry of Materials, Vol. 17, No. 24, 29.11.2005, p. 6198-6204.

    Research output: Contribution to journalArticle

    @article{e2c8c8834b634ddfa6f8b9af3518f6cd,
    title = "Preparation of organic-inorganic hybrids possessing nanosheets with perovskite-related structures via exfoliation during a sol-gel process",
    abstract = "Organic-inorganic hybrids containing exfoliated nanosheets with a perovskite-related structure have been prepared from an n-decoxy derivative of an ion-exchangeable layered perovskite, HLaNb2O7· xH2O (HLaNb) or HCa2Nb3O10· xH2O (HCaNb), silanol-terminated poly(dimethylsiloxane) (PDMS), and tetramethoxysilane (TMOS) via a sol-gel process involving the reaction of the n-decoxy derivative with a PDMS-TMOS mixture and subsequent intentional hydrolysis with hydrochloric acid. The X-ray diffraction (XRD) patterns of the resultant products after intentional hydrolysis indicate both preservation of the perovskite-like slab structure and disappearance of stacking order. Partial exfoliation of layered perovskites is correspondingly observed by transmission electron microscopy (TEM). The formation of a polysiloxane network composed of PDMS chains and Qn units ((RO)4-nSi(OSi)n: R = H, CH3) via intentional hydrolysis is shown by the solid-state 29Si CP/MAS (cross-polarization and magic angle spinning) NMR spectroscopy. These products are expected to possess the Nb-O-Si linkage interface since a signal assignable to the (SiO)Si(CH3) 2O-Nb environment is present in the 29Si CP/MAS NMR spectra of products prepared from an n-decoxy derivative of HLaNb (or HCaNb), PDMS, and TMOS in a similar manner without intentional hydrolysis and the Nb-O-Si bonds are expected to be preserved during hydrolysis. The exfoliated structures should be formed during the intentional hydrolysis process since the products prepared without intentional hydrolysis clearly exhibit a stacking order along the c axis.",
    author = "Seiichi Tahara and Yosuke Takeda and Yoshiyuki Sugahara",
    year = "2005",
    month = "11",
    day = "29",
    doi = "10.1021/cm0514793",
    language = "English",
    volume = "17",
    pages = "6198--6204",
    journal = "Chemistry of Materials",
    issn = "0897-4756",
    publisher = "American Chemical Society",
    number = "24",

    }

    TY - JOUR

    T1 - Preparation of organic-inorganic hybrids possessing nanosheets with perovskite-related structures via exfoliation during a sol-gel process

    AU - Tahara, Seiichi

    AU - Takeda, Yosuke

    AU - Sugahara, Yoshiyuki

    PY - 2005/11/29

    Y1 - 2005/11/29

    N2 - Organic-inorganic hybrids containing exfoliated nanosheets with a perovskite-related structure have been prepared from an n-decoxy derivative of an ion-exchangeable layered perovskite, HLaNb2O7· xH2O (HLaNb) or HCa2Nb3O10· xH2O (HCaNb), silanol-terminated poly(dimethylsiloxane) (PDMS), and tetramethoxysilane (TMOS) via a sol-gel process involving the reaction of the n-decoxy derivative with a PDMS-TMOS mixture and subsequent intentional hydrolysis with hydrochloric acid. The X-ray diffraction (XRD) patterns of the resultant products after intentional hydrolysis indicate both preservation of the perovskite-like slab structure and disappearance of stacking order. Partial exfoliation of layered perovskites is correspondingly observed by transmission electron microscopy (TEM). The formation of a polysiloxane network composed of PDMS chains and Qn units ((RO)4-nSi(OSi)n: R = H, CH3) via intentional hydrolysis is shown by the solid-state 29Si CP/MAS (cross-polarization and magic angle spinning) NMR spectroscopy. These products are expected to possess the Nb-O-Si linkage interface since a signal assignable to the (SiO)Si(CH3) 2O-Nb environment is present in the 29Si CP/MAS NMR spectra of products prepared from an n-decoxy derivative of HLaNb (or HCaNb), PDMS, and TMOS in a similar manner without intentional hydrolysis and the Nb-O-Si bonds are expected to be preserved during hydrolysis. The exfoliated structures should be formed during the intentional hydrolysis process since the products prepared without intentional hydrolysis clearly exhibit a stacking order along the c axis.

    AB - Organic-inorganic hybrids containing exfoliated nanosheets with a perovskite-related structure have been prepared from an n-decoxy derivative of an ion-exchangeable layered perovskite, HLaNb2O7· xH2O (HLaNb) or HCa2Nb3O10· xH2O (HCaNb), silanol-terminated poly(dimethylsiloxane) (PDMS), and tetramethoxysilane (TMOS) via a sol-gel process involving the reaction of the n-decoxy derivative with a PDMS-TMOS mixture and subsequent intentional hydrolysis with hydrochloric acid. The X-ray diffraction (XRD) patterns of the resultant products after intentional hydrolysis indicate both preservation of the perovskite-like slab structure and disappearance of stacking order. Partial exfoliation of layered perovskites is correspondingly observed by transmission electron microscopy (TEM). The formation of a polysiloxane network composed of PDMS chains and Qn units ((RO)4-nSi(OSi)n: R = H, CH3) via intentional hydrolysis is shown by the solid-state 29Si CP/MAS (cross-polarization and magic angle spinning) NMR spectroscopy. These products are expected to possess the Nb-O-Si linkage interface since a signal assignable to the (SiO)Si(CH3) 2O-Nb environment is present in the 29Si CP/MAS NMR spectra of products prepared from an n-decoxy derivative of HLaNb (or HCaNb), PDMS, and TMOS in a similar manner without intentional hydrolysis and the Nb-O-Si bonds are expected to be preserved during hydrolysis. The exfoliated structures should be formed during the intentional hydrolysis process since the products prepared without intentional hydrolysis clearly exhibit a stacking order along the c axis.

    UR - http://www.scopus.com/inward/record.url?scp=28944448950&partnerID=8YFLogxK

    UR - http://www.scopus.com/inward/citedby.url?scp=28944448950&partnerID=8YFLogxK

    U2 - 10.1021/cm0514793

    DO - 10.1021/cm0514793

    M3 - Article

    AN - SCOPUS:28944448950

    VL - 17

    SP - 6198

    EP - 6204

    JO - Chemistry of Materials

    JF - Chemistry of Materials

    SN - 0897-4756

    IS - 24

    ER -